Structural Studies of Bi2O3âNaPO3 Glasses by Solid State Nuclear

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Structural Studies of Bi2O3-NaPO3 Glasses by Solid State Nuclear Magnetic Resonance and X-ray Photoelectron Spectroscopy Ruili Zhang, Jinjun Ren, Xinqiang Yuan, Yun Cui, Lei Zhang, and Long Zhang J. Phys. Chem. C, Just Accepted Manuscript • DOI: 10.1021/acs.jpcc.7b01871 • Publication Date (Web): 24 Apr 2017 Downloaded from http://pubs.acs.org on May 2, 2017

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The Journal of Physical Chemistry

Structural Studies of Bi2O3-NaPO3 Glasses by Solid State Nuclear Magnetic Resonance and Xray Photoelectron Spectroscopy

Ruili Zhanga,b, Jinjun Rena*, Xinqiang Yuana, Yun Cuia, Lei Zhanga , Long Zhanga*

a

Key Laboratory of Materials for High Power Laser, Shanghai Institute of Optics and Fine

Mechanics, Chinese Academy of Sciences, Shanghai 201800, China b

University of Chinese Academy of Sciences, Beijing 100039, China

ABSTRACT: Glasses in the system xBi2O3–(100-x)NaPO3 were prepared using transitional melting−quenching and characterized using solid state nuclear magnetic resonance (SSNMR), xray photoelectron spectroscopy (XPS), and Fourier-transform infrared spectroscopy (FT-IR). The addition of Bi2O3 results in the depolymerization of the phosphorus chain and the formation of Q(n) (n = 0, 1, 2) phosphorus species, where n represents the number of P-O-P bonds that can be quantified using

31

P magic angle spinning (MAS) NMR and constant-time double-quantum

based dipolar recoupling effects nuclear alignment reduction (CT-DQ-DRENAR). The 23

Na{31P},

31

P{23Na}, and XPS results consistently prove that both Na+ and Bi3+ ions are

bounded by phosphorus tetrahedron [PO4]3-. Unlike other trivalent ions such as Ga3+ and Al3+, which connect with the phosphorus tetrahedron by corner-sharing, Bi3+ ions were first proved to

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share edge with the phosphorus tetrahedron by the analysis of

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P spectra, taking the charge

balance and bond valance consideration into account. Such a difference in connectivity results in significant structural differences.

1. INTRODUCTION Bismuth has attracted extensive attention in the past decades owing to its unique properties such as a low photon energy, high non-linear optical properties, tunable broad luminescence covering the ultraviolet to near infrared region. Such properties make bismuth useful in broad applications such as in extended infrared transmission,1-3 optical switches,4-7 luminescence sensitizers,8-10 infrared optical amplifiers, and lasers11-15. Bismuth exists in multiple oxidation states such as 0, +1, +2, +3, and +5 in different hosts. The oxidation state and optical properties, such as absorption and luminescence, strongly depend on the local structure of bismuth.16-20 Phosphate glasses are widely used in optical communications, solid lasers, optical switching devises, and three dimensional (3D) displays because of their high solubility with active metal ions.21-24 Despite this considerable interest, a fundamental understanding of the properties on the basis of the structural organization of these glasses has not been achieved. Solid-state nuclear magnetic resonance (SSNMR) spectroscopy has been proven to be a powerful tool in addressing structural issues, especially for disordered materials, owing to its well-proven ability to provide local structural information.25-27 Furthermore, X-ray photoelectron spectroscopy (XPS) provides valuable information on structural elucidation. In the present contribution, we carried out a combined multinuclear NMR and XPS investigation of bismuth phosphate glasses in the system xBi2O3–(100-x)NaPO3. These glasses were originally reported by Daviero et al.28 and the coordination shells of Bi3+ was mainly studied. Single and double resonance NMR experiments have been used to characterize the local environments of the sodium, bismuth, and phosphorus species, whereas XPS has been employed to examine the bond connectivity. On the basis of spectroscopic results as well as charge balance and bond valance considerations, we developed a comprehensive and quantitative structural model describing the local structure, polyhedral connectivity, the connectivity between Bi3+ and phosphorus tetrahedron [PO4]3-, and the distribution of Na+ ions.

2. EXPERIMENTAL SECTION


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Sample Preparation and Characterization. All the xBi2O3‒(100-x)NaPO3 glasses (x = 0, 5, 10, 12.5, 15, and 17.5) were prepared by the conventional melt-quenching technique, using Bi2O3 and NaPO3 (aladdin, purity > 99.9%) as the starting materials. The powdered materials were thoroughly mixed and heated in a platinum crucible for 20 min at temperatures ranging from 800 °C to 950 °C, depending on the compositions. The melt was then rapidly poured onto a steel plate. The amorphous nature of the samples was verified using X-ray powder diffraction (XRD) with a filtered Cu Kα radiation in Bragg-Brentano geometry on a PANalytical Empyrean (Netherlands) diffractometer (diffraction angle range of 10o ≤ 2θ ≤ 80o; See Figure S1 in the Supporting Information). Differential thermal analysis (DTA) was employed using a SII TG/DTA 7300 DTA instrument (Seiko Co., Japan) with a heating rate of 10 K/min. The DTA curves are shown in Figure S2 (See the Supporting Information). At room temperature, infrared (IR) transmittance spectra in the range of 400–1400 cm-1 were collected using a Fouriertransform infrared spectrometer (FT-IR) (Nicolet 6700, Thermo Nicolet, America) with the KBr pellet method. Solid State NMR. All the NMR experiments were carried out at ambient temperature on a Bruker Avance III HD 500M spectrometer (11.7 T). In all the experiments, a reproducible stationary magnetization was created by a saturation comb sequence.

31

P single pulse magic

angle spinning (MAS) experiments were performed at resonance frequencies of 202.5 MHz using a 4 mm MAS NMR probe operated at a spinning rate of 12 kHz. 90o pulse length of 4.5 µs was used. Recycle delays were chosen as 256 s. The

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P chemical shifts were calibrated with

85% H3PO4 solution, using NH4H2PO4 (= 1.12 ppm) as the secondary reference. Line shape analysis and deconvolution were performed with the DMFIT software package.29 To investigate the spatial distribution of phosphorous species,

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P constant-time double-

quantum based dipolar recoupling effects nuclear alignment reduction based on BABA-xy16 pulse blocks (31P-CT-DQ-DRENAR- BABA-xy16)30 experiments were carried out on a 2.5 mm MAS probe at a spinning rate of 27 kHz. 90o pulse lengths of 3.6 µs were used with a recycle

delay of 90 s. The signal intensity difference, (S0− S′ )/S0 (corresponding to the signal

amplitudes without (S0) and with (S′) dipolar recoupling effects) was measured as a function of

the dipolar mixing time, NTr. It can be approximated by a simple parabola:30


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6 − ′ = (1 + 2!) (1) ( ) 5

where θ is the phase rotation angle (0o ≤ 2θ ≤ 360o) in discrete steps at fixed mixing times

and #∑ is the effective dipolar coupling constant between nuclei k and the observed nuclei j.

This quantity can be used to characterize the average homonuclear dipole-dipole coupling strength, independent of the order and geometry of the spin systems. 23

Na isotropic chemical shifts and second-order quadrupolar effect (SOQE) values were

measured at 132.3 MHz using 2D triple quantum MAS (TQMAS) NMR with three-pulse zfiltering sequence.31, 32 A spinning rate of 12.0 kHz was used. In the 23Na TQMAS experiments, the first two hard pulses (5.8 and 1.9 µs in length) and the third soft pulse (10 µs) were transmitted at radio frequency amplitudes corresponding to the liquid-state nutation frequencies of 56.2 kHz and 12.3 kHz, respectively. The evolution time was incremented by 10.42 µs and 45 increments were recorded. The “second order quadrupolar effects” (SOQE = CQ(1 + η2/3)1/2, with CQ and η corresponding to the nuclear electric quadrupolar coupling constant and the electric field gradient asymmetry parameter, respectively) and the isotropic chemical shifts, δcsiso were obtained by comparing the centers of gravity of the projections in the isotropic F1 and anisotropic F2 dimensions. In order to assess the dipole interactions between

23

Na and

31

P, rotational echo double

resonance (REDOR) experiments were carried out using the pulse sequence of Gullion and Schaefer.33 In the 23Na{31P} REDOR measurements, a compensation scheme described by Chan and Eckert34 was used to correct the effects of small pulse imperfections. 23Na{31P} compensated REDOR experiments were carried out with 180o pulse lengths of 7.9 µs and 7.8 µs for 23Na and 31

P, respectively. A relaxation delay of 0.5 s was employed. Dipolar second moments, M2SI (S =

23

Na, I =

31

P) were extracted by a parabolic analysis of the initial part of the experimental

REDOR curves (S/S0 ≤ 0.2) using the formula:35, 36

∆ 4 = )*+ ( ) (2) 3(

This quantity can be used to characterize the average dipole-dipole coupling strength, independent of the order and geometry of the spin systems.


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P{23Na} REDOR experiments were performed with 180o pulse lengths of 8.2 µs and 7.9

µs for

31

P and

23

Na, respectively. A relaxation delay of 90 s was employed. For

23

Na (spin

quantum number of 3/2), the analysis of the REDOR data in the limit of short evolution times was performed using the expression:33

∆ 1 (2 + 18-))*+ ( ) (3) = 15(

where the efficiency factor f (0 ≤ f ≤ 1) accounts for the extent to which the dipolar coupling of spin I in the noncentral Zeeman states with the observed spins, S influences the REDOR response.37, 38 The efficiency factor, f is estimated from the experimental

23

Na SOQE

results and simulated REDOR curves using the SIMPSON program package.39 The obtained M2 values can be compared with the calculated results based on structural models using the wellknown van Vleck equation:40 )*+ =

4 / 45 . 0 ( + 1)1+ 1* ℏ 3+* (4) 15 4( *

where γ+ and γ* are the gyromagnetic ratios of nuclear I and S involved, and r+*

corresponds to the internuclear distance.

XPS Measurements. XPS measurements were carried out using a Thermo Fisher Scientific X-ray photo-electron spectroscope using Al Kα radiation (1486.6 eV) with ultrahigh vacuum (pressure 10 mol%,


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2 + ?@ AB ⟹ 2 ()

(D)

2 + ?@ AB ⟹ 2 (D)

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()

(6)

NMR and XPS results have consistently proved that both Bi3+ and Na+ ions are bounded by phosphorus tetrahedrons. Bi3+ ions have no effect on the average distribution of Na+ ions around the phosphorus tetrahedrons. No Bi-O-Na and Bi-O-Bi connectivity exist in these glasses. Bi3+ ions act as glass modifiers to neutralize the negative charge of phosphorus tetrahedrons [PO4]3-. According to the charge balance requirements, all the three phosphorus species, Q(2)0Bi, Q(1)1Bi, and Q(0)2Bi should be electrically neutral or the total glass will not be electrically neutral. In the Q(1)1Bi and Q(0)2Bi species, Bi3+ ions should afford +1 and +2 charges, respectively to keep electrically neutral. The total charges afforded by Bi3+ to compensate the charge of phosphorus tetrahedron can be calculated according to the fractions of the three phosphorus species obtained from the deconvolution of the

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P spectra using the formula {[Q(1)1Bi]+2 [Q(0)2Bi]}×(100-x),

where [Q(1)1Bi], [Q(0)2Bi], and x are the fractions of Q(1)1Bi, Q(0)2Bi species and the added content of Bi2O3, respectively. Theoretically, it should be equal to 6x, which corresponds to the total positive charge of all Bi3+ ions added in the form of Bi2O3. Figure 9 shows the comparison between them. Both these values are very close to each other, which proves the validity of the charge balance calculation.


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(2)

Q

0Bi (1)

100

Q

1Bi (0)

Q

80 Fraction (%)

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60


2Bi

60 40 20 0 -2

0

2

4

6

8 10 12 Bi2O3mol%

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16

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Figure 8. Dependence of phosphorus species on the Bi2O3 content.


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100 Charge number

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60

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80 60 40 20 0 0

2

4

6

8 10 12 Bi2O3 mol/%

14

16

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Figure 9. Comparisons between the charge numbers calculated based on the added Bi2O3 content (black squares) and the charge numbers calculated according to the fraction of 31P spectra (red circles). The error bars indicate an error of 10%.

Although both the alloyed oxides are trivalent, the Bi2O3–NaPO3 glasses are quite different from the Ga2O3–NaPO3 glasses. In Ga2O3–NaPO3 glasses, Ga3+ ions contribute + 0.5 ~ + 0.75 charge to the phosphorus species Q(1)1Ga, dependent on the coordinate number.42 The contributed charge can be calculated using formula

E:FGHIG J:G

IKKL>H:>KH HMNOG

. In Q(0)2Ga species, the contributed

charges are twice of that in Q(0)1Ga. However, different with Ga3+ ions, Bi3+ ions contribute +1 and +2 charges to the Q(1)1Bi and Q(0)2Bi species, respectively, in Bi2O3–NaPO3 glasses although Bi3+ exists as six coordination28, which is double the values calculated according to the above formula. To meet the requirements of the double charge, the P-O-Bi bonds should be edgesharing in these glasses. In edge-sharing structure, one Bi3+ connects with two O2- of [PO4]3-, equivalent to form two P-O-Bi bonds (see Figure 10), and thus results in the double charge contribution as that in corner-sharing like P-O-Ga bonds. Such an edge-sharing of P-O-Bi can be


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found in crystalline Na3Bi(PO4)244. However, only the corner-sharing of P-O-Ga is found in crystalline Na3GaP8O2345.

Figure 10. Structure sketches of phosphorus species in 10Bi2O3–90NaPO3 and 10Ga2O3– 90NaPO3 glasses. Such connectivity difference can be found from

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P spectra (see Figure 11). It illustrated

that the signal fraction from Q(1)1Bi is much bigger than that from Q(1)1Ga. This is because in this composition bismuth reacting with phosphorus only form Q(1)1Bi , but the Ga3+ can form multiple species such as Q(1)1Ga, Q(1)2Ga, Q(2)1Ga with phosphorus (see figure 18 in ref. 42). In cornersharing connectivity, since only one oxygen of phosphorus tetrahedron is participated in the connectivity, the phosphorus species have chance to connect with different number of Ga3+ ions and form multiple phosphorus species. However, in edge-sharing since two oxygens are occupied, such chance is limited. From above analysis we can find that it is possible to judge the connectivity between glass modifiers and glass formers is edge-sharing or corner-sharing, just simply based on the deconvolution of 31P spectra and charge balance calculation.


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10

0

-10 -20 (ppm)

-30

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-40

Figure 11. 31P spectra of 10M2O3–90NaPO3 glass. (M = Ga (up) and Bi (bottom))

To the best of our knowledge, this is the first time to distinguish edge-sharing and cornersharing structure in phosphate glass by NMR. As in the Ga2O3–NaPO3 and Bi2O3–NaPO3 glasses, such different connectivity will result in huge structural difference. It is important to distinguish these two different connectivities since great property differences could be related with them. It will promote a deeper insight of glass structures.

5. CONCLUSIONS In summary, this work developed quantitative local structure study on bismuth sodium metaphosphate glasses with the composition of xBi2O3–(100-x)NaPO3. Alloying Bi2O3 into NaPO3 results in the depolymerization of phosphorus chain of NaPO3 and the evolution of phosphorus species in the process of Q(2)0Bi→ Q(1)1Bi→ Q(0)2Bi. The SSNMR and XPS results have consistently proved that both the Bi3+ and Na+ ions are bounded by phosphorus tetrahedrons. No linkage was formed between them. The addition of Bi2O3 has not changed the average distribution of Na+ ions around the phosphorus tetrahedron. Different with Ga3+ ions which connect with phosphorus tetrahedrons by corner-sharing, Bi3+ ions share edges with the phosphorus tetrahedrons, as confirmed based on the deconvolution of the 31P spectra and charge balance calculations. To the best of our knowledge, we first used such simple method to


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distinguish edge-sharing and corner-sharing structure in phosphate glasses. Such method will promote a deeper insight of glass structures.

ASSOCIATED CONTENT Supporting Information The Supporting Information is available free of charge on the ACS Publications website at DOI:……….. XRD patterns and DTA curves.

AUTHOR INFORMATION *Corresponding author. E-mail: [email protected] (J. Ren); *corresponding author: Email: [email protected] (L. Zhang) Notes: The authors declare no competing financial interest

ACKNOWLEDGMENTS This work was supported by the National Natural Science Foundation of China with the grant number NSFC 61475174, NSFC 61675218 and 100 Talents Program of Chinese Academy of Sciences.

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(43) Ren, J.; Eckert, H. Quantification of Short and Medium Range Order in Mixed Network Former Glasses of the System GeO2−NaPO3: A Combined NMR and X-ray Photoelectron Spectroscopy Study. J. Phys. Chem. C 2012, 116, 12747-12763. (44) Diouri, M.; Drache, M.; Abraham, F.; Wignacourt, J. P. Phase transitions in the Na3PO4BiPO4 system, Phase Transit. 1988, 13, 23-28. (45) Palkina, K. K.; Maksimova, S. I.; Chibiskova, N. T.; Chudinova, N. N.; Karmanovsk,N. B. Double Ultraphosphates Na3M(III)P8O23 (M(III): Ga, Al). Neorg. Mater. 1993, 29, 119-120.


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Structural Studies of Bi2O3âNaPO3 Glasses by Solid State Nuclear

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Structural Studies of Bi2O3âNaPO3 Glasses by Solid State Nuclear