本研究探討160-180℃在高壓釜中合成Sn1-xSbxS(x=0.00, 0.02, 0.04, 0.06)與270℃於油胺中合成Cu2(Co1.1-xZnx)SnS4(x=0, 0.2, 0.4, 0.6, 0.8, 1.1)試料的相生成及可調控能隙之研究。SnS、Sn0.98Sb0.02S試料分別在160℃反應12小時與180℃反應24小時可得到orthorhombic SnS純相，顯示Sb的摻入提高了orthorhombic SnS相的活化能。Sb在SnS中的固溶度約5.4 at%。. SnS形貌為300-700 nm，厚度約30-40 nm的奈米板狀晶粒。Sn1-xSbxS(x= 0.02, 0.04, 0.06)試料尺寸會隨著Sb濃度增加而減小。藉由提升Sb的濃度至5.4 at%，Sb-doped SnS奈米晶之能隙可由1.30調控至1.39 eV。將Sn0.96Sb0.04S薄膜在氮氣中以200℃退火，其能隙值無變化，而當退火溫度為300和350℃，能隙值由1.35eV減小至1.33與1.31 eV，此現象可由退火造成Sb與S在試片中的蒸發來解釋。
以溶熱法在油胺中於270℃反應24小時合成Cu2CoSnS4合金，以醋酸鈷為前軀體優於硝酸鈷與氯化鈷前軀體，其可促進純和合乎計量比的Cu2CoSnS4奈米晶生成，推論醋酸根離子可當作螯合基，平衡油胺中各陽離子的反應性。在本研究中，Cu2(Co1-xZnx)SnS4奈米晶的生長速率較Cu2CoSnS4與Cu2ZnSnS4奈米晶為慢，這可能是合成Cu2(Co1-xZnx)SnS4奈米晶時，鈷離子和鋅離子與其他陽、陰離子反應時會彼此競爭，阻礙對方進入晶格，而降低CCZTS奈米晶生長的速率。Cu2(Co1.1-xZnx)SnS4(x=0, 0.2, 0.4, 0.6, 0.8, 1.1)試料能隙值由1.21 eV分別增加為1.25、1.28、1.31、1.37、1.46 eV。此結果可能為Cu2CoSnS4與Cu2ZnSnS4價帶與導帶結構分別混合所致。本研究顯示可調控能隙之Sn1-xSbxS與Cu2(Co1-xZnx)SnS4奈米晶有應用於光伏元件的潛力。

SUMMARY

In the present study, phase formation and tunable bandgaps of Sn1-xSbxS (x = 0.00, 0.02, 0.04, 0.06), and Cu2(Co1.1-xZnx)SnS4 (x = 0.0, 0.2, 0.4, 0.6, 0.8, 1.1) samples synthesized at 160-180˚C in teflon-lined stainless steel autoclave and at 270˚C in oleylamine (OLA), respectively, were explored. The substitution solubility of Sb in SnS was about 5.4 at%. The bandgap of Sn1-xSbxS nanocrystals can be tuned from 1.30 to 1.39 eV by increasing the Sb concentration to about 5.4 at%. On annealing in N2, the bandgap of 200˚C-annealed Sn0.96Sb0.04S films remained unchanged, while that of 300- and 350˚C-annealed Sn0.96Sb0.04S films decreased from 1.35 to 1.33 and 1.31 eV, respectively. This result can be explained in terms of evaporation of Sb and S during annealing.
On solvothermal synthesis of Cu2CoSnS4 alloys at 270˚C for 24 h in OLA, the Co(CH3COO)2 precursor was superior to CoCl2 and Co(NO3)2 precursors in enhancing the growth of pure and stoichiometric Cu2CoSnS4 nanocrystals. In the present study, the growth rate of Cu2(Co1-xZnx)SnS4 nanocrystals was less than that of Cu2CoSnS4 and Cu2ZnSnS4 nanocrystals. For Cu2(Co1.1-xZnx)SnS4 (x = 0.0, 0.2, 0.4, 0.6, 0.8, 1.1) samples the bandgap increased from 1.21 to 1.25, 1.28, 1.31, 1.37, and 1.46 eV, respectively. This result may be explained in terms of the hybridization of valence and conduction bands of Cu2CoSnS4 and Cu2ZnSnS4. The Sn1-xSbxS and Cu2(Co1-xZnx)SnS4 nanocrystals with tunable bandgap may be promising candidates for photovoltaic applications.

Key words : Sn1-xSbxS nanocrystals、Cu2(Co1-xZnx)SnS4 nanocrystals、one-pot system、tunable bandgap

INTRODUCTION

Currently, the Cu2-II-IV-VI4 compounds such as Cu2ZnSnS4 (CZTS), and Cu2ZnSnSe4 (CZTSe), the IV-VI compounds such as SnS, and SnSe containing non-toxic and abundant elements have drawn great attention as alternatives to Cu(In,Ga)Se2 for use as the solar cell absorber layer. To maximize the conversion efficiency, the band gap of an ideal PV absorber layer should be around 1.3 eV for the single-junction cell and 1.0-1.9 eV for the two-junction cell. These requirements can be achieved by tunning the bandgaps of PV materials via adjusting the chemical compositions.
Recently, few studies about the tunable bandgaps of SnS and CZTSe were reported. further exploration on the synthesis and characterization of cation-doped IV-VI compounds and Cu2-II-IV-VI4 compounds are still attractive. In the present study, the tunable bandgap of Sn1-xSbxS nanocrystals and Cu2(Co1-xZnx)SnS4 alloys were explored.

MATERIALS AND METHODS

For Sn1-xSbxS nanocrystals, a mixture of SnCl2∙2H2O, Na2S∙9H2O, and SbCl3 powders were dissolved in ethylene glycol and then stirred for 2 h. The solutions were loaded into a 40 ml teflon-lined stainless steel autoclave and then heated at 160-180˚C for 12-24 h followed by slow cooling to room temperature, respectively. The product was centrifuged and then washed with deionized water and ethanol to remove the dissoluble by-product, and finally dried at about 50℃.
For Cu2(Co1-xZnx)SnS4 alloys, a mixture of CuCl, Co(CH3COO)2∙2H2O, Zn(CH3COO)2∙2H2O, SnCl4∙5H2O, CH4N2S powders was dissolved in OLA with magnetic stirring, and then heated at 270˚C in N2 for 24-48 h. The product was centrifuged and then washed with hexane and ethanol to remove the dissoluble by-product, and finally dried at about 50℃.
The microstructure of samples was observed using SEM and TEM. The chemical compositions of samples were measured with SEM/EDS and TEM/EDS. The phases in the samples were analyzed using XRD and Raman spectrometer. The optical properties of samples were characterized using diffuse absorbance and reflectance UV-vis spectrometer. The valence states of the chemical elements in the samples were measured using XPS.

RESULTS AND DISCUSSION

Sn1-xSbxS (x = 0.00, 0.02, 0.04, 0.06, 0.08, 0.10) powders with single orthorhombic SnS (JCPD 00-039-0354) were synthesized in an autoclave at 160-180°C for 12-24 h as shown in Fig. 2, where the XRD (111) peak of Sn1-xSbxS (x = 0.02, 0.04, and 0.06) powders shifts to a higher diffraction angle with the extent increasing with the Sb concentration as compared with that of the SnS sample. Sn and Sb in the Sn1-xSbxS samples are in the oxidation state of 2+ and 3+, respectively, from XPS measurement. The substitution of Sb for Sn reduces the lattice constant of SnS because the ion radius of Sb3+, 0.076 nm, is smaller than that of Sn2+, 0.093 nm. However, no further shift in the XRD peaks of Sn1-xSbxS (x = 0.08, 0.10) powders was observed, revealing that there may have a limit in the substitution solubility of Sb in the SnS lattice. In the present study, the substitution solubility of Sb in SnS is about 5 at% which is comparable to that for the Sb-doped SnS thin films reported previously
Sn1-xSbxS (x = 0.00, 0.02, 0.04, 0.06) films are in the range of 1.30-1.39 eV, which are obtained from their reflectance spectra by performing the Kubelka-Munk transformation
The Cu2(Co1-xZnx)SnS4 (x=0.0, 0.2, 0.4, 0.6, 0.8, and 1.1) samples were synthesized at 270˚C for 24-48 h to obtain pure Cu2(Co1-xZnx)SnS4 phase which was characterized by the sharp Raman peaks. The Raman spectra of Cu2(Co1-xZnx)SnS4 (x=0.0, 0.2, 0.4, 0.6, 0.8, and 1.1) showing that main peaks shift from CCTS (326 cm-1) to CZTS (335 cm-1). The direct bandgaps of Cu2(Co1-xZnx)SnS4 (x = 0.0, 0.2, 0.4, 0.6, 0.8, and 1.1) samples are 1.21, 1.25, 1.28, 1.31, 1.37, and 1.46 eV, which are obtained from their absorbance spectra, showing that the direct bandgaps increase with the Zn concentrations linearly.

CONCLUSION

SnS and Sn1-xSbxS (x = 0.00, 0.02, 0.04, 0.06) powders with single orthorhombic SnS phase (JCPD 00-039-0354) were synthesized in ethylene glycol at 160-180 °C for 12-24 h, respectively. The maximum substitution solubilities of Sb in SnS were about 5 at%. The bandgaps of Sn1-xSbxS nanocrystals could be tuned in the range of 1.30-1.39 eV. For the Sn0.96Sb0.04S film subjected to annealing in N2 the bandgaps of 200°C-annealed ones remained nearly unchanged, while those of 300- and 350°C-annealed ones decreased with the annealing temperature because of the evaporation of Sb and S. In the present study, the Sn1-xSbxS nanocrystals with tunable bandgap may be the potential candidates as the photovoltaic materials.
On solvothermal synthesis of Cu2CoSnS4 alloys at 270˚C for 24 h in OLA, the Co(CH3COO)2 precursor was superior to CoCl2 and Co(NO3)2 precursors in enhancing the growth of pure and stoichiometric Cu2CoSnS4 nanocrystals. One can suggest that the acetate anion may behave as a chelating ligand, and thus balance the reactivities of various cations in the OLA solvent. In the present study, the growth rate of Cu2(Co1-xZnx)SnS4 nanocrystals was less than that of Cu2CoSnS4 and Cu2ZnSnS4 nanocrystals. It seems that during synthesis of Cu2(Co1-xZnx)SnS4 nanocrystals a competition between Co and Zn cations for reaction with other cations and anion (S2-) may hinder each other from incorporation into the lattice, and thus delay their growth rate. For Cu2(Co1.1-xZnx)SnS4 (x = 0.0, 0.2, 0.4, 0.6, 0.8, 1.1) samples the bandgap increased from 1.21 to 1.25, 1.28, 1.31, 1.37, and 1.46 eV, respectively. This result may be explained in terms of the hybridization of valence and conduction bands of Cu2CoSnS4 and Cu2ZnSnS4. The Sn1-xSbxS and Cu2(Co1-xZnx)SnS4 nanocrystals with tunable bandgap may be promising candidates for photovoltaic applications.

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