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Structural, Spectroscopic, and Magnetic Studies on Copper Tartrate Crystals

  • S. Ariponnammal EMAIL logo and R. Velvizhi
Published/Copyright: March 27, 2019
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Zeitschrift für Naturforschung A
From the journal Zeitschrift für Naturforschung A Volume 74 Issue 9

Abstract

Copper tartrate crystals were grown by the gel growth method and characterised by energy-dispersive X-ray (EDAX), scanning electron microscopy, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV-vis spectroscopy, Fourier transform infrared, photoluminescence (PL), electron paramagnetic resonance, and low-temperature magnetic studies in the temperature range 300–20 K. The XRD study confirmed the orthorhombic structure of the crystal and the XPS study established the Cu2+ ions in the crystal. UV-vis study deduced the energy gap as 2.15 eV, confirming the semiconducting nature, and Urbach energy as 0.4686 eV. PL showed the presence of Cu2+ vacancy-related defects. Low-temperature magnetic study confirmed the paramagnetic nature in the temperature range 300–77 K, and the crystal showed a weak ferromagnetic signal at 20 K, which is interesting. The magnetic field along with the low temperature caused an ordered spin orientation.

Keywords: Copper Tartrate; Low-Temperature Magnetic Study; X-ray Diffraction

1 Introduction

Tartrate crystals have applications as dielectric, ferroelectric, and piezoelectric materials. They also show non-linear optical properties. They are used in transducers as well as linear and non-linear mechanical devices [1], [2], [3]. The manganese tartrate crystal is temperature-sensitive and used to measure temperature. Zinc tartrate forms a bright coating and used as protection for metals [4]. Some tartrate crystals are used for controlling laser emission [5], [6], [7], [8], [9]. Several tartrate compounds find applications in medical, pharmaceutical, and industrial fields. It is notable that tartrates are used in the treatment of cognitive disorders associated with diabetes, cancer, and herpes [10], [11], [12]. Iron tartrate plays an important role as contrast blocks of renal tissues prior to their dehydration [13]. Iron tartrate is present in apple juice as one of its main constituents [14]. Certain tartrate compounds find applications in cosmetics as hair conditioner additives and tanning agents for skin [15], [16]. Light causes a change in colouration in copper tartrate [17]. Copper tartrate has been shown to stimulate the luteinizing hormone in vitro [18]. So, the study on tartrate compounds seems to be application-oriented, and therefore the copper tartrate crystal was chosen for the present work.

2 Materials and Methods

Copper tartrate (CuC4H4O6) crystals were grown by the gel growth method in silica gel in pure form. All chemicals were of analytical grade and used without further purification. First, a 1 M sodium metasilicate solution was added to a 1 M tartaric acid solution in a U tube until the pH value reached 4.5. Once gelled, a 1 M aqueous solution of copper chloride was poured on top of the gel (along the walls of the tube to avoid any gel breakage) and allowed to diffuse into the gel. Thus, pure copper tartrate crystals of bluish green colour were grown (Fig. 1).

Figure 1: Crystals of copper tartrate grown by the gel growth method.
Figure 1:

Crystals of copper tartrate grown by the gel growth method.

The equation for the chemical reaction during gel growth for the formation of the crystal is

CuCl2+C4H6O6→CuC4H4O6+2HCl

The grown copper tartrate crystals were characterised by scanning electron microscopy (SEM), energy dispersive X-ray (EDX), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV-vis spectroscopy, photoluminescence (PL), Fourier transform infrared (FTIR), electron paramagnetic resonance (EPR), and low-temperature magnetic studies. The SEM images were recorded on a scanning electron microscope (JEOL model JSM-6390, Japan). The EDX spectrum was recorded on an Oxford Incapentax3 instrument (England). Powder XRD was performed by a Richseifert diffractometer. The charge valence of copper was studied by a Thermo Fisher Scientific XPS instrument with Al Kα radiation (1486.6 eV). The UV-vis absorption spectrum was recorded on a Perkin Elmer model Lamda 35 spectrophotometer in the spectral range 200–900 nm. The PL emission spectrum was recorded on a Shimadzu spectrofluorophotometer (Model RF-5301PC) employing a 150 W Xe lamp as the excitation source. The FTIR spectrum was recorded using a Perkin Elmer spectrum BX model spectrophotometer by the KBr pellet technique in the range 400–4000 cm−1 at a resolution 2 cm−1. The EPR spectrum of the Cu(II) ion in the copper tartrate crystal was recorded with a Bruker model EMX plus spectrometer at room temperature. The low-temperature magnetic measurements were conducted by a Lakeshore model VSM 7410 vibrating sample magnetometer.

3 Results and Discussion

3.1 Energy Dispersive X-ray Analysis

The energy dispersive X-ray spectrum of the copper tartrate is shown in Figure 2. It is seen that Cu and O are present in 49.24 and 50.76 wt.% and 19.63 and 80.37 at.%. The apparent concentration of Cu and O is 42.10 and 77.51, respectively.

Figure 2: EDAX pattern of copper tartrate.
Figure 2:

EDAX pattern of copper tartrate.

3.2 Scanning Electron Microscopy

The SEM image of copper tartrate (CuC4H4O6) at the magnification of ×55,000 is shown in Figure 3. It shows a weak, uniform distribution of nearly triangular-type particles with the particle size of 87 nm. The triangular morphology is highlighted in Figure 3 by triangles. The particles are embedded in a rock-like structure. It resembles a coral rock-like structure because it was grown by the gel growth method. Figure 3 also shows clearly the appearance of the particles as coral flowers.

Figure 3: SEM image of copper tartrate at ×55,000 magnification.
Figure 3:

SEM image of copper tartrate at ×55,000 magnification.

3.3 X-ray Powder Diffraction

The powder XRD pattern of copper tartrate is shown in Figure 4. The peaks are indexed by the method of least-squares fit from the XRD data (Table 1). The crystal is found to be crystallised in the orthorhombic structure with lattice parameters a = 8.441 ± 0.01 Å, b = 12.611 ± 0.02 Å, c = 8.883 ± 0.02 Å, α = 90°, β = 90°, and γ = 90°, which are in agreement with the reported values [http://iucr.sdsc.edu/iucr-top/17/iucr/abstracts/so558]. The JCPDS card number is 01-0158.

Figure 4: XRD pattern of copper tartrate.
Figure 4:

XRD pattern of copper tartrate.

Table 1:

Parameters deduced from XRD data.

Copper tartrated-spacing (Å)Rel. int. (%)hkl
Molecular formula: CuC4H4O67.646100.00011
7.13111.46110
Cu Kα radiation λ =1.5418 Å5.89371.42020
4.64323.03002
Structure: orthorhombic4.37137.13121
 a = 8.441 ± 0.01 Å4.08228.53210
 b = 12.611 ± 0.02 Å3.84424.51102
 c = 8.883 ± 0.02 Å3.76736.74130
 V = 945.59 Å33.51439.89220
 α = 90°3.30612.99221
3.0565.55032
 β = 90°2.92425.00003
2.55510.21240
 γ = 90°2.44018.63321

3.4 X-ray Photoelectron Spectroscopy

The copper 2p scan electron binding energy spectrum of copper tartrate is shown in Figure 5. The spectrum consists of spin-orbit-split 2p3/2 and 2p1/2 peaks and satellites. These peaks seem to be sensitive in deducing the charge valence of copper ions in copper tartrate. The peaks 2p3/2 and 2p1/2 observed at 938.6 and 958.4 eV, respectively, in Figure 5 are ascribed to the Cu2+ ions [19]. The Cu 2p peak has a significantly split spin-orbit component with Δ = 19.8 eV. A broad satellite peak is observed near 945.2 eV. It has been reported that strong satellite peaks appear in the XPS spectrum of transition-metal elements with unpaired electrons, but not for a closed-shell structure. In other words, Cu+ (d10) configuration does not show satellite peaks and Cu2+ (d9) shows such peaks. Therefore, the observed satellite peak at 945.2 eV is ascribed to Cu2+ ions [20], [21]. Moreover, it has been reported that for transition metals, the absence of the satellite peaks is the fingerprint for elemental or diamagnetic lines. The occurrence of prominent satellites corresponds to the existence of the paramagnetic state [22], [23], [24], [25]. This confirms the paramagnetic state of the copper tartrate crystal.

Figure 5: XPS spectrum of Cu 2p scan of copper tartrate.
Figure 5:

XPS spectrum of Cu 2p scan of copper tartrate.

The oxygen 1s scan electron binding energy spectrum of copper tartrate is shown in Figure 6. The spectrum consists of the 1s peak at about 537.6 eV, which is ascribed to carbon with oxygen [19]. The carbon 1s scan electron binding energy spectrum of copper tartrate is shown in Figure 7. It shows the 1s peak at about 292.3 eV, which is ascribed to carbonyl, that is, carbon with oxygen [21].

Figure 6: XPS spectrum of O 1s scan of copper tartrate.
Figure 6:

XPS spectrum of O 1s scan of copper tartrate.

Figure 7: XPS spectrum of C 1s scan of copper tartrate.
Figure 7:

XPS spectrum of C 1s scan of copper tartrate.

3.5 UV-visible Spectroscopy

The absorbance spectrum of copper tartrate recorded in the UV-vis region is shown in Figure 8. It shows higher absorption in the UV region (at about 200 nm) than in any other region of the spectrum. This makes the material suitable for devices requiring good absorption of UV radiation, such as UV filters. The spectrum shows high transmittance in the visible region. The wide transmission in the entire visible region (300–900 nm) makes it a potential candidate for optoelectronic applications.

Figure 8: UV-visible spectrum of copper tartrate.
Figure 8:

UV-visible spectrum of copper tartrate.

The plot of (αhγ)1/2 versus energy is shown in Figure 9. The energy gap is deduced as 2.15 eV. It also shows that it is an indirect band gap material. Generally, the energy gap of a semiconductor lies below 3 eV [26]. This confirms the semiconducting nature of the copper tartrate crystal. It has been reported that the colour of a crystal also gives a hint as to whether the crystal is an insulator or a semiconductor. Semiconductor crystals are mostly coloured, whereas insulator crystals are colourless, transparent, and clear. To be very clear, a semiconductor crystal can have no strong electronic or vibronic transitions in the visible region (740–360 nm or 1.7–3.5 eV) [27]. It is notable that the crystals in the present case are coloured. They exhibit no strong electronic or vibronic transitions in the visible spectral region between 740 and 360 nm. This confirms the nature of the copper tartrate crystal as a semiconductor. The Urbach plot of copper tartrate is shown in Figure 10. The Urbach energy is deduced as 0.4686 eV.

Figure 9: Plot of (αhγ$\upalpha\textit{h}\upgamma$)1/2 versus energy.
Figure 9:

Plot of (αhγ)1/2 versus energy.

Figure 10: Urbach plot of copper tartrate.
Figure 10:

Urbach plot of copper tartrate.

3.6 Photoluminescence

Figure 11 shows the PL spectrum of copper tartrate at the excitation wavelength of 250 nm at room temperature. Copper is a transition-metal impurity. It is a fast diffuser and gives rise to both radiative and non-radiative centres. The PL spectrum comprises two bands of which one sharp green emission is observed at 509.7 nm and another weak red emission is observed at 766.8 nm. These emissions originate from Cu2+ vacancy-related defects or their complexes. The green Cu emission has been extensively studied by Shinoya and co-workers [28].

Figure 11: PL spectrum of copper tartrate.
Figure 11:

PL spectrum of copper tartrate.

3.7 Fourier-Transform Infrared Spectroscopy

Figure 12 shows the FTIR spectrum of the copper tartrate and Table 2 presents the observed absorption frequencies and their assignments in relation to their characteristic vibrational modes. The broad trough observed between 3646 and 2025 cm−1 corresponds to the O-H bond, which confirms the hydrous nature of the compound. The bands at 884.7, 819.4, 743.3, 645.4, 493.1, and 427.8 cm−1 observed in the fingerprint region between 1000 and 400 cm−1 are characteristic bands of the metal ion complex.

Figure 12: FTIR spectrum of copper tartrate.
Figure 12:

FTIR spectrum of copper tartrate.

Table 2:

Assignment of the FTIR bands of copper tartrate.

S. No.Frequency (cm–1)Assignments [28], [26], [29]
13419.3O-H stretching
23354.0O-H stretching
33092.9O-H stretching
42973.3O-H stretching
52788.4O-H stretching
62636.1O-H stretching
72559.9O-H stretching
82364.1O-H stretching
91624.4C-O stretching
101439.5O-H stretching
111330.7C-O stretching
121232.8C-O stretching
131069.6C-O stretching
14884.7Cu(II) complex
15819.4Cu(II) complex
16743.3Cu(II) complex
17645.4Cu(II) complex
18493.1Cu(II) complex
19427.8Cu(II) complex

3.8 Electron Paramagnetic Resonance

The EPR spectrum of copper tartrate is shown in Figure 13. Copper(II) has S = 1/2 and nuclear spin I = 3/2. A group of four lines is expected per complex [30]. In any general orientation, the number of such resonance lines will provide the number of distinguishable complexes in the host lattices. The 3d9 ion of Cu(II) shows four lines from a single complex. However, it displays a broad EPR line resonance centred at g = 2.16 with line width ΔH = 59 G. The EPR line is a very intense, broad line since copper is in high concentration. It conceals four hyperfine lines.

Figure 13: EPR spectrum of copper tartrate.
Figure 13:

EPR spectrum of copper tartrate.

3.9 M-H curve

The magnetic properties of copper tartrate were analysed by the M-H curve shown in Figure 14 at temperatures 273, 200, 150, 77, and 20 K. Copper is a transition-metal group element and exists in both Cu+ and Cu2+ configurations. In Cu+, the electronic configuration is 3d10 and does not have any unpaired electron. But in Cu2+, the electronic configuration of copper is 3d9 with one unpaired electron. So, it is expected to show paramagnetic behaviour [31]. Numerous magnetic studies have been made on different materials, and it has been reported [32], [33] that magnetic susceptibility of mixed iron-lead levo tartrate crystals have paramagnetic nature. Investigation of copper chloride hydroxide hydrate [Cu3Cl4(OH)2 ⋅ 2H2O] has shown the interesting behaviour of a weak ferromagnetic signal at 17.5 K [33]. Similar to this, in the present study, Cu in copper tartrate is in the Cu2+ state. It shows the expected paramagnetic behaviour up to 77 K. However, below 77 K (at 20 K) it shows a weak ferromagnetic behaviour as shown in Figure 15, which is interesting. The applied field of 15,000 G is large enough to align almost all the available copper spins. The magnetic moment is found to decrease with the increase of temperature. Low temperature along with magnetic field brings the crystal to a more ordered state.

Figure 14: Merged field-dependent magnetisation curves for copper tartrate at various temperatures (273, 200, 150, 77, and 20 K).
Figure 14:

Merged field-dependent magnetisation curves for copper tartrate at various temperatures (273, 200, 150, 77, and 20 K).

Figure 15: M-H curve of copper tartrate at 20 K.
Figure 15:

M-H curve of copper tartrate at 20 K.

4 Conclusions

Copper tartrate crystals were grown by the gel Growth method. EDX analysis showed that the weight percentages of Cu and O are in agreement with the expected values. The SEM image showed a weak, uniform distribution of nearly triangular-type particles embedded in a coral rock-like structure with particle size 87 nm. XRD analysis confirmed the orthorhombic structure of the crystal. UV-vis study showed that the material is suitable for UV filters and optoelectronic applications. The energy gap was deduced as 2.15 eV, confirming the semiconducting nature, and the Urbach energy was deduced as 0.4686 eV. The PL spectrum comprised two bands, one sharp green emission and another weak red emission due to the presence of Cu2+ vacancy-related defects or their complexes. FTIR confirmed the presence of the copper metal ion complex. The EPR spectrum displayed a very intense, broad EPR line concealing four hyperfine lines since copper is in high concentration. It has a resonance centred at g = 2.16 with line width ΔH = 59 G. The M-H curve of copper tartrate confirmed its paramagnetic behaviour up to 77 K. Below 77 K, that is, at 20 K, it showed a weak signal of interesting ferromagnetic behaviour. Low temperature along with magnetic field brings the crystal to a more ordered state.

Acknowledgement

The authors are thankful to IIT Madras, Chennai, for access to their low-temperature facilities.

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Received: 2018-11-07
Accepted: 2019-03-03
Published Online: 2019-03-27
Published in Print: 2019-09-25

© 2019 Walter de Gruyter GmbH, Berlin/Boston

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  2. General
  3. Electrical Conductivity of Magnesium Oxide/Molten Carbonate Eutectic Coexisting System
  4. Atomic, Molecular & Chemical Physics
  5. Quintet States 1s2s2p2 5P and 1s2p3 5So for Be-Like Systems
  6. Graphene-Based Waist-Enlarged Optical Fibre Sensor for Measurement of Sucrose Concentration
  7. Dynamical Systems & Nonlinear Phenomena
  8. Three-Soliton Interaction and Soliton Turbulence in Superthermal Dusty Plasmas
  9. Delta Shock Wave in a Perfect Fluid Model with Zero Pressure
  10. Magnetoacoustic Nonlinear Solitary and Freak Waves in Pair-Ion Plasma
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  12. Shock Wave Kinematics in a Relaxing Gas with Dust Particles
  13. Quantum Theory
  14. An Improved Ping-Pong Protocol Using Three-Qubit Nonmaximally Nonorthogonal Entangled States
  15. Solid State Physics & Materials Science
  16. Structural, Spectroscopic, and Magnetic Studies on Copper Tartrate Crystals
  17. Features of Electrical and Photoelectric Properties of GaS(Yb) Monocrystals
  18. Insight into the Structural, Electronic, Elastic, Mechanical, and Thermodynamic Properties of XReO3 (X = Rb, Cs, Tl) Perovskite Oxides: A DFT Study
https://doi.org/10.1515/zna-2018-0498
Keywords for this article
Copper Tartrate; Low-Temperature Magnetic Study; X-ray Diffraction

Articles in the same Issue

  1. Frontmatter
  2. General
  3. Electrical Conductivity of Magnesium Oxide/Molten Carbonate Eutectic Coexisting System
  4. Atomic, Molecular & Chemical Physics
  5. Quintet States 1s2s2p2 5P and 1s2p3 5So for Be-Like Systems
  6. Graphene-Based Waist-Enlarged Optical Fibre Sensor for Measurement of Sucrose Concentration
  7. Dynamical Systems & Nonlinear Phenomena
  8. Three-Soliton Interaction and Soliton Turbulence in Superthermal Dusty Plasmas
  9. Delta Shock Wave in a Perfect Fluid Model with Zero Pressure
  10. Magnetoacoustic Nonlinear Solitary and Freak Waves in Pair-Ion Plasma
  11. Hydrodynamics
  12. Shock Wave Kinematics in a Relaxing Gas with Dust Particles
  13. Quantum Theory
  14. An Improved Ping-Pong Protocol Using Three-Qubit Nonmaximally Nonorthogonal Entangled States
  15. Solid State Physics & Materials Science
  16. Structural, Spectroscopic, and Magnetic Studies on Copper Tartrate Crystals
  17. Features of Electrical and Photoelectric Properties of GaS(Yb) Monocrystals
  18. Insight into the Structural, Electronic, Elastic, Mechanical, and Thermodynamic Properties of XReO3 (X = Rb, Cs, Tl) Perovskite Oxides: A DFT Study
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