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Vol. 5. Num. 3.
Pages 199-292 (July - September 2016)
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Vol. 5. Num. 3.
Pages 199-292 (July - September 2016)
Original Article
DOI: 10.1016/j.jmrt.2015.11.003
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Photoluminescence and semiconducting behavior of Fe, Co, Ni and Cu implanted in heavy metal oxide glasses
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Mohamed A. Marzouka,
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marzouk_nrc@yahoo.com

Corresponding author.
, Sherief M. Abo-Nafa, Hamdia A. Zayedb, Nevien S. Hassanc
a Glass Research Department, National Research Centre, Giza, Egypt
b Physics Department, Faculty of Girls, Ain-Shams University, Cairo, Egypt
c Egyptian Organization for Standardization and Quality (EOS), Cairo, Egypt
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Table 1. Calculated optical parameters of the prepared glasses.
Abstract

Transition metal ions (0.5wt%) of Fe2O3, CoO, NiO or CuO doped heavy metal oxide glasses having chemical composition of 60PbO·20Bi2O3·20MxOy mol% (where MxOy=B2O3 or SiO2 or P2O5) were prepared by conventional melt annealing method. Combined optical and photoluminescence properties have been measured and employed to evaluate the prepared glassy samples. From the absorption edge data, the values of the optical band gap Eopt, Urbach energy (ΔE) and refractive index were calculated to estimate semiconducting behavior. Photoluminescence and values of the optical energy gap were found to be dependent on the glass composition. The variations of the photoluminescence intensity, values of optical band gap, Urbach energy and refractive index gave an indication to use the prepared glasses for design of novel functional optical materials with higher optical performance.

Keywords:
Glass
Heavy metal
Transition metal
Photoluminescence
Band gap
Urbach energy
Full Text
1Introduction

Transition metals doped glasses have found an interest in many areas of application. Such glasses are good materials for use in optical, electric, thermal, and mechanical applications. Transition metal ions are characterized by partially filled d-shell that can frequently exist in a number of oxidation states and the electro-optical behavior can occur as a result of electron transfers from ions in a lower to those in a higher oxidation state [1]. Many studies [1–3] have pointed out the relationships between the structure of the host glass and the properties of the doped ions that, in turn, help for designing of glasses for different applications. The current interest in transition metal or rare earth ions doped glasses is mainly for two reasons: firstly, their well defined and sharp energy levels may serve as structural probes for the environment of the dopant, and secondly, the modifications of the energy level structure of the rare earth ions caused by the glassy environment may lead to interesting applications [1,3]. Recently, heavy metal oxides such as Bi2O3 and PbO have been added to the conventional glass systems in order to enhance the optical and mechanical behavior. Bismuth-doped glasses show various emission centers at wavelengths ranging from 400 to 2500nm [4,5]. Therefore, these glasses are very promising optical materials for photonic as well as optoelectronic applications. The transition metals doped bismuth glasses show enhanced photoluminescence. These enhanced photoluminescence were observed due to energy transfer mechanism from the above ionic species to bismuth. In addition, bismuth containing glasses are used in the electronic field due to the low field strength and high polarizability of Bi3+ ions [6]. This property makes these glasses very useful in optical memory devices.

In the present work, iron, cobalt, nickel and copper ions, implanted in host lead and bismuth heavy metal oxide glasses, were doped with low amounts of common glass formers, i.e. borate, silicate and phosphate. UV–visible absorption and photoluminescence were determined for the prepared glasses. It is also very important to investigate optical band gap and the refractive index to detect the semiconducting behavior of such glasses.

2Experimental details2.1Preparation of glasses

The glasses were prepared from chemically pure materials. Orthoboric acid (H3BO3) was used for B2O3, SiO2 was introduced as pulverized quartz, P2O5 was introduced in the form of NH4H2PO4, Pb3O4 was used for PbO and Bi2O3 was introduced as such. Transition metals (Fe2O3, CoO, NiO or CuO) were added (0.5wt%) in the form of their respective oxides to the base undoped lead bismuth borate, silicate and phosphate. The accurately weighed batches having chemical composition of 60PbO–20Bi2O3–20MxOy mol% (where MxOy=B2O3 or SiO2 or P2O5) were melted in alumina crucibles at 1150–1200°C for 1h to achieve homogeneous and clear samples. The crucibles were rotated at intervals to promote chemical and physical homogeneity of the melts. After complete fining, the melts were cast into warmed stainless steel molds of required dimensions. The prepared glasses were immediately transferred to a muffle furnace regulated at 350°C for annealing. After 1h, the muffle furnace, with the glasses inside, was left to cool down to room temperature at a rate of 25°C/h.

2.2UV–visible absorption spectra

Optical (UV–visible) absorption spectral measurements were performed using an UV-VIS spectrophotometer (type T80, PG Instruments, England). The range of measurement was from 200 to 1100nm. Perfectly polished samples of the dimensions 1cm×1cm×0.2cm were measured twice to confirm the accuracy of the absorption peaks. The irradiated glasses were immediately measured after the irradiation process.

2.3Photoluminescence spectra

Photoluminescence emission spectra were recorded at room temperature using a fluorescence spectrophotometer type (Jasco FP-6500, Japan) equipped with a xenon flash lamp as the excitation light source. The scan speed is 0.1s step−1 with a step length of 0.25nm and a slit width of 0.2nm.

2.4Optical band gap energy (Eopt) and Urbach energy (ΔE)

There are two types of optical transitions: direct and indirect. They can occur at the fundamental absorption edge of crystalline and non-crystalline semiconductor.

In both cases, electromagnetic waves interact with the electrons in the valence band, which are raised across the fundamental gap to the conduction band [7]. In order to determine the optical band gap for such glasses, Mott and Davis [8] have suggested the following expression for the relation between the optical band gap, absorption coefficient and energy (hv) of the incident photon:

where Eopt is the optical energy gap, B is a constant called the band tailing parameter and n is an index which can be assumed to have values of 1/2, 3/2, 2 and 3, depending on the nature of the electronic transition responsible for the absorption. n=1/2 for allowed direct transition, n=3/2 for forbidden direct transition and n=3 for forbidden indirect transition, with n=2 refers to indirect allowed transitions [9].

Using the above Eq. (1), by plotting (αhν)1/2 as a function of photon energy , one can find the optical energy band gaps (Eopt) for indirect transition.

The Urbach energy gives the width of the tails of the localized states within the optical band gap [10]. The dependence of the absorption coefficient in the region of lower photon energy of the absorption edge can be described by the following formula [11]:

where B is the constant, ΔE is the Urbach energy and v is the frequency of radiation. Plots were also drawn between ln(α) and (Eq. (2)) and from these plots, the value of the Urbach energy ΔE can be calculated from the reciprocal of the slope of the linear portion of such plots.

The refractive index, n, can be calculated from the value of Eg using the formula proposed by Dimitrov and Sakka [12] as follows:

3Results and discussion3.1UV–visible absorption spectra

Figs. 1–4 illustrate the UV–visible absorption spectra of Fe2O3, CoO, NiO or CuO doped lead bismuth borate, silicate and phosphate glasses, respectively. According to our previous study [13], the undoped glasses show three UV absorption bands at about 235, 305 and 390nm and an intense near-visible at about 435nm. The observed strong UV absorption spectral bands from all studied glasses are primarily due to absorption of ferric (Fe3+) ions present as trace impurities beside extra bands within the UV near visible region in the prepared glasses from the sharing absorption spectra of Pb2+ and Bi3+ ions in the UV-near visible region [14–18].

Fig. 1.

Absorption spectra of Fe-doped glasses.

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Fig. 2.

Absorption spectra of Co-doped glasses.

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Fig. 3.

Absorption spectra of Ni-doped glasses.

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Fig. 4.

Absorption spectra of Cu-doped glasses.

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The optical spectrum of transition metal ions doped glasses can be summarized as follows.

3.1.1Fe2O3 doped glasses

Fig. 1 illustrates the UV–visible absorption spectra of Fe2O3-doped glasses, which reveal three strong and broad UV absorption band centered at about 240, 305 and 355nm, followed by a broad asymmetrical near-visible band centered at about 445nm. The band at 445nm is resolved due to the addition of 0.5% of Fe2O3 as dopant to the composition of the host glass, indicating its relationship to ferric ions (Fe3+) added, and is assigned to the transitions 6A1g(S)4A1g(G)+4Eg(G) [19].

3.1.2CoO doped glasses

Fig. 2 represents the UV–visible absorption spectra of CoO-doped glasses, which reveal three strong and broad UV absorption band centered at about 240, 310 and 360nm. This is followed by a very broad three visible absorption peaks at 448, 536 and 630nm. The observed visible peaks are related to the presence of cobalt ions in the divalent state in two coordinations, the octahedral is identified at about 450nm and the tetrahedral coordination at about 536 and 630nm. The presence of two coordination states at the same time can be related to the similarity of the ligand stabilization energies of the two coordination states as reported by several authors [14,15,20].

3.1.3NiO doped glasses

Fig. 3 shows the UV–visible absorption spectra of NiO-doped glasses, which reveal three strong and broad UV absorption band centered at about 240, 305 and 370nm. The extended visible absorption band at about 820nm can be attributed to the presence of Ni2+ ions (3d8 configuration) of spin allowed transition 3A2g(3F)3T1g(3F) [21,22].

3.1.4CuO doped glasses

Fig. 4 depicts the UV–visible absorption spectra of CuO-doped glasses, which reveal three strong and broad UV absorption band centered at about 240, 305 and 355nm. The absorption broad band centered at 794nm is related to the divalent copper ions (Cu2+) in octahedral coordination and is assigned to the 2B1g2B2g transition of Cu2+ ions [14,15,20].

3.2Photoluminescence spectra

Heavy metal bismuth ions doped conventional glass formers exhibit two characteristic emission peaks centered at about 465 and 550nm which is usually attributed to 1S03P0 or 3P2 (spin forbidden) or 1S03P1 or 1P1 (spin–orbit coupling transitions) [13].

Figs. 5–8 show the emission spectra of heavy metal oxide glasses containing low concentrations of borate, silicate and phosphate glass formers, and doped with Fe2O3, CoO, NiO or CuO. The observed emission spectra, at 220nm excitation, show two strong emission bands at about 462 and 550nm for iron, nickel and copper doped glasses, while CoO doped glasses possess one emission band centered at about 462nm. The intensity of the emission bands was found to be dependent on both of the type of glass former and the transition metal ion.

Fig. 5.

Emission spectra of Fe2O3-doped glasses.

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Fig. 6.

Emission spectra of CoO-doped glasses.

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Fig. 7.

Emission spectra of NiO-doped glasses.

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Fig. 8.

Emission spectra of CuO-doped glasses.

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3.2.1Photoluminescence spectra of Fe2O3 doped glasses

The emission spectra of 0.5% Fe2O3-doped samples, excited at 220nm (in Fig. 5), show two strong broad emission bands extending nearly from 435 to 625nm in the visible light range; the first emission peak is centered at 466nm, and the other is centered at 555nm.

It is accepted that iron can exist in glasses in two valences, namely Fe2+ and Fe3+, and the ratios of them depend on the glass composition and conditions of melting [10,23]. It is well-known that the visible luminescence, related to deep level emissions, mainly results from defects such as interstitials and oxygen vacancies. According to Manjari et al. [24] the spectra of Fe(III) ions exhibit two emission bands which are: a strong UV emission band at 373nm and a relatively weak blue emission band at 450nm, which are assigned to the transitions 4T2g(D)6A1g(S) and 4A1g(G)6A1g(S), respectively.

3.2.2Photoluminescence spectra of CoO doped glasses

The emission spectra of 0.5% CoO-doped samples, excited at 220nm (in Fig. 6), show only one strong broad emission band centered at about 462nm.

It is fairly accepted that cobalt exists in glasses mostly in the divalent state with two coordinations, namely the octahedral and tetrahedral ones [10,23]. The Co2+ ion has a d7 electronic configuration and in a tetrahedral crystal field presents the splitting of the energy levels of a d3 electronic configuration in an octahedral field. In octahedral coordination (Co2+) free ion ground state 4F splits into the 4T1, 4T2 and 4A2 states with the 4T1 state as the lowest one. In a tetrahedral symmetry, the energy levels of Co2+ ions are 4T2(4F), 4T1(4F), 2E(2G) and 4T1(4P), etc., with the ground state of 4A2(4F). The emission band of Co2+ ions in the region 600–700nm is assigned to 2E(2G)4A2(4F) of Co2+ ions in tetrahedral coordination [21,25,26].

According to Naresh et al. [27] Co-doped glasses exhibited two emission bands of Co-doped glasses in the visible region which were attributed to 4T1(4P)4A2(4F) and 4T1(4P)4T2(4F) tetrahedral transitions of Co2+ ion.

Therefore, it is accepted that the origin of the emission bands of Co-doped glasses can be related not only to the presence of transition metal ion cobalt but also to the effect of heavy metal ions. Previous study [13] showed that the heavy metal ion Bi3+ is a very promising luminescent material and its emission peak is not located in one characteristic spectral region but varies from the ultraviolet region into the red region with differing host glass matrix. Bismuth doped borate, phosphate and silicate exhibit fluorescence emission centered at about 400nm [13]. Consequently, the emission peak observed in the present results at 462nm in case of CoO-doped glasses can be ascribed to Bi3+ ions matching with those attributions mentioned in Ref. [13].

3.2.3Photoluminescence spectra of NiO doped glasses

The emission spectra of 0.5% NiO-doped glasses, excited at 220nm (in Fig. 7), show three strong broad emission bands centered at about 464, 548 and 560nm.

Ni2+ ions (3d8) are expected to exist as octahedral and tetrahedral coordination sites within the glass matrix [10,23]. Furthermore, the energy levels of the excitation states of Ni2+ are different with the matrices change. The luminescence of Ni2+ ions doped glasses could be associated with the d–d optical transitions. It was reported [21,25,28] that energy levels of Ni2+ ions in octahedral symmetry are 3A2g(F)4T2g(F), 3A2g(F)3T1g(F) and 3A2g(F)3T1g(P). In addition to these three spin allowed transitions, a spin forbidden transition 3A2g(F)1Eg(D) can be observed.

Many authors [21,25,28] have proposed that the luminescence properties of Ni-doped glasses exist in two regions, which are the green (577nm) and red (670nm) regions. Hence, according to the energy levels of Ni2+ ions transitions in octahedral sites, the emissions in green and red regions are assigned to the 1T2g(D)3A2g(F) and 1T2g(D)3T2g(F) transitions.

3.2.4Photoluminescence spectra of CuO doped glasses

The emission spectra of 0.5% CuO-doped glasses, excited at 220nm (in Fig. 8), show two strong broad emission bands extending from 425 to 600nm in the visible light range; the first emission peak is centered at 464nm and the other is centered at 556nm. According to the octahedral crystal field, the Cu2+ (3d9) loses its degeneracy and splits into 2Eg and 2T2g with 2Eg being the lower level. The luminescence spectra of CuO-doped glasses exhibit emission peaks at 420, 520 and 630nm, which are assigned to 3d94s3d10 triplet transitions in Cu2+ ions [29–33].

4Optical band gap (Eopt), Urbach energy (ΔE) and refractive index

Figs. 9–12 show the plots for indirect band gap of the prepared glasses. Energy gap and Urbach energy values are listed in Table 1. The values of optical mobility gap (Eopt) of iron, cobalt, nickel and copper ions doped glasses in the present work were found to be changeable within the range 2.444–1.490eV. Table 1 reveals characteristic values of optical band gap, which are changeable between borate, silicate and phosphate containing glasses. The calculated values of ΔE of the present glass systems are observed to be within the range of 0.125–0.89eV for all the glasses. Mott and Davis [8] reported that, for amorphous materials to be semiconductor, ΔE values should lie between 0.045 and 0.67eV. The recorded values of ΔE for both of the CoO and CuO-doped glasses, and NiO-doped silicate and phosphate reveal Urbach's energy values that are close to those of the semiconductors. Fe2O3-doped glasses and NiO-doped borate glass have not matched Mott and Davis [8] postulation. The variation of Eopt and ΔE could be attributed to the network structural differences brought about by the existence of transition metal ions in different oxidation or coordination states [34].

Fig. 9.

Optical band gap of Fe2O3-doped glasses.

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Fig. 10.

Optical band gap of CoO-doped glasses.

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Fig. 11.

Optical band gap of NiO-doped glasses.

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Fig. 12.

Optical band gap of CuO-doped glasses.

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Table 1.

Calculated optical parameters of the prepared glasses.

SampleBorateSilicatePhosphate
Eopt (eV)  ΔE (eV)  n  Eopt (eV)  ΔE (eV)  n  Eopt (eV)  ΔE (eV)  n 
Fe  2.433  0.890  2.569  2.390  0.790  2.584  2.242  0.711  2.638 
Co  1.594  0.660  2.937  1.579  0.590  2.945  1.490  0.250  2.998 
Ni  2.335  0.749  2.603  2.035  0.386  2.721  1.801  0.257  2.827 
Cu  2.444  0.610  2.565  2.314  0.125  2.611  2.200  0.368  2.654 

The values of the refractive index thus obtained for all the glass samples are given in Table 1. The average value of refractive index, n, shows noticeable dependence on glass composition. The observed results indicate a slight successive increase in the refractive index from the borate to silicate to phosphate matrices. Generally, the increase of refractive index can be attributed to large atomic weight and coordinate number of Bi2O3 and the high polarizability of the Bi3+ ions in the glass system.

5Contribution of the effect of transition metal ions and Bi2O3 on the photoluminescence and semiconducting behavior

It can be pointed out that bismuth doped borate, phosphate and silicate exhibit fluorescence emission centered at about 400nm, which is attributed to the 3P11S0 transition of Bi3+ ions [35–37]. The transition metal ions show enhanced photoluminescence of the studied heavy metal oxide glasses. This enhanced photoluminescence observed is due to energy transfer mechanism for both of the transition metal ion and Bi3+ from the ionic species of bismuth. It is also evident that the presence of high percent of PbO (60mol%) and Bi2O3 (20mol%) suppresses the effects of the 3d transition metal ions in their normal environments and, hence, they did not sharply or distinctly impart their known characteristics bands as they normally exhibit in alkali borate, alkali silicate, lead borate and lead silicate glasses [24–26,38].

The variation of Eopt and ΔE could be attributed to the network structural differences brought about by the existence of transition metal ions in different oxidation or coordination states. The transition metal ions enhance the non-bridging oxygens (NBOs) concentration and the states originating from NBOs are more easily excited than that of bridging oxygen atoms. Therefore, the increase in concentration of the NBO ions results in the shifting of valence band to higher energies and reduces the band gap energy [39]. From the comparison between all glass network formers, it is evident that the addition of Bi2O3 enhances the formation of octahedral groups, resulting in a highly cross-linked network, and thus causes the variations in the optical mobility gap between borate, silicate and phosphate glasses [2,18].

6Conclusions

In the present study, transition metal ions of Fe2O3, CoO, NiO or CuO doped heavy metal oxide glasses having chemical composition of 60PbO·20Bi2O3·20MxOy (where MxOy=B2O3 or SiO2 or P2O5) were prepared by conventional melt annealing method. Photoluminescence and semiconducting properties have been measured and employed to evaluate the prepared glassy samples. The transition metal doped samples show strong UV-near visible bands that are related to the presence of Pb2+ and Bi3+ beside extra characteristic bands due to the respective transition metal ions. The observed emission spectra, recorded at 220nm excitation, show two strong broad emission bands at about 462 and 550nm for all glasses except CoO-doped glasses. The transition metal ions show enhanced photoluminescence of the studied heavy metal oxide glasses. Semiconducting behavior was found to be related to the type of transition metal ion and the glass network former existed in the glasses. The variation of Eopt and ΔE could be attributed to the network structural differences brought about by the existence of transition metal ions in different oxidation or coordination states. The increase of the refractive index can be attributed to large atomic weight and coordinate number of Bi2O3 and the high polarizability of the Bi3+ ions in the glass system.

Conflicts of interest

The authors declare no conflicts of interest.

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