Preparation,characterization and luminescence of (SBA-15)-Ag 2 S nanocomposite material

Abstract

SBA-15 mesoporous molecular sieve was prepared using triblock copolymer poly (ethylene glycol)-block-poly (propylene glycol)-block (poly ethylene glycol) as the template, tetraethyl orthosilicate as the silica source in acidic medium. Through toluene/water two-phase interface, nano Ag₂S guest has been synthesized. By thermal diffusion method, (SBA-15)-Ag₂S host-guest nanocomposite material was prepared. The results of powder X-ray diffraction (XRD) showed that the silver sulfide assembled did not destroy the molecular sieve skeleton and the host-guest nanocomposite prepared still maintained good crystallinity. Infrared spectra showed that the host molecular sieve skeleton in the composite material was intact. Transmission electron microscopic results showed that the pores of SBA-15 after loading of Ag₂S were obvious and not damaged. The nitrogen adsorption-desorption results at 77 K showed that the guest has already partly occupied the molecular sieve pores, which led to the decrease in the pore volume and specific surface area to some extent. UV-Vis reflection spectra showed that Ag₂S molecules were well assembled into SBA-15 and the molecules presented a highly dispersed state. The luminescent research results showed that the (SBA-15)-Ag₂S nanocomposites after the encapsulation have luminescent phenomena and the luminescence is stronger than that of the Ag₂S. The (SBA-15)-Ag₂S nanocomposites have obvious emission peaks at 425 nm, which has a potential applied prospect as a light emitting diode etc optical material.

Keywords

Nanocomposite material SBA-15 mesoporous molecular sieve luminescence

1 Introduction

In recent years, nanosulfides have become a hot research field due to their unique physical and chemical properties, which have raised great concerns because of the huge development potential and applied value in electronics [1], photocatalysis [2, 3], ceramic [4], biological and medical fields [5]. Semiconductor nano sulfides have shown the applicant prospect in the fields of catalysis, sensing, optics, magnetics and batteries because of its unique physical and chemical properties. The preparation of metal sulfide nanomaterials, the study of their growth mechanism, and further the regulation of their size, the adjustment and control for morphology and physical properties are of great significance to the deep study of the relationship between structure and physical properties, and ultimately to the design and synthesis for functional materials according to people’s wishes [6 –8]. Since Fujishima et al. [9] discovered the semiconductor materials with photocatalytic properties in 1972, as nanostructured semiconductor metal sulfides have unique physical and chemical properties, it made the studies of this kind of materials more and more focus, such as CuS [10, 11], ZnS [12, 13], CdS [14, 15]. Silver sulfide nanomaterials as important optical and electric function materials, have a broad applied value in many fields, such as photoelectrical conductors, photovoltaic cells, ionic conductors, infrared detections and so on [16 –18]. Ag₂S as one kind of narrow band semiconductor luminescent materials of I – VI group with high chemical stability, has been widely used in photocell photoconductor device, infrared detector, fast ion conductor manufacturing industry. Nano Ag₂S, because of larger specific surface, produced a significant quantum size effect, making it in the light absorption and sensing, catalysis and many fields exhibit special properties different from bulk materials. In recent years, people found it also have very strong ability to sterilize, thus in the aspects of biology, medicine and environment and so forth more important potential application will also exist. In 1998, Zhao et al. [19] synthesized ordered mesoporous SBA-15 molecular sieve, which has a lot of advantages like regular sized pores and large specific surface. SBA-15, as one of mesoporous materials, has several advantages of easy synthesis, highly ordered hexagonal arrangement of pores, large pore size (8–30 nm), the thick pore wall, high mechanical strength, high specific surface area and good hydrothermal stability. Due to high surface area and the good pore size distribution, mesoporous SBA-15 material recently has been widely used in loading catalyst [20, 21], polymer [22, 23], drug [24, 25], metal [26] and semiconductor nano materials [27], with a practical prospect as catalysts and adsorbent materials [28] and others. To the best of our knowledge, no report on nano mesoporous molecular sieve material-silver sulfide nanocomposite preparation, characterization and its properties studies was seen. In this study, SBA-15 was synthesized in acidic medium and nano Ag₂S was synthesized in two phase mixture of toluene and water [29]. Then (SBA-15)-Ag₂S was synthesized by thermal diffusion method using (SBA-15) as host material and the Ag₂S as guest material. XRD, Fourier transform infrared (FT-IR) spectroscopy, N₂ adsorption-desorption, transmission electron microscopy (TEM), UV-Vis diffusion reflectance spectra and luminescence study were used to characterize the prepared materials. Thereby, the structural characteristics of composite materials and luminescent performance are explored.

2 Experimental

2.1 Reagent and instrument

The reagents for the preparation of SBA-15 include: Pluronic triblock copolymer, poly (ethylene glycol)-block-poly (propylene)-poly (ethylene glycol) was purchased from Sigma-Aldrich, USA (P₁₂₃: average molecular weight 5800). Tetraethylorthoxysilicate (TEOS) and hydrochloric acid were obtained from Beijing Chemical Plant, China.

The reagents for the synthesis of nano Ag₂ S include: Silver nitrate and sulfocarbamide were the products of Sinopharm Chemical Reagent Co., Ltd. Sodium oleate and methylbenzene were purchased from Beijing Chemical Plant, China. Unless otherwise specified, all reagents were of analytical grade.

A magnetic agitator (Jintan Kexi Instrument Manufacturing Co. Ltd., China) and high speed centrifuge (Beijing Medical Centrifuge Factory, China) were used in the experiments.

2.2 Synthesis of SBA-15 molecular sieve

2 g of tri-block copolymer poly (ethylene glycol)-block-poly (propylene glycol)-block (poly ethylene glycol) was dissolved in 15 g of deionized water and 60 g of 2 mol/L HCl solution and magnetically stirred. At the same time, 4.25 g of TEOS was slowly added and a homogeneous solution was formed. The initial optimum molar ratio of the amount of each material was (P₁₂₃: TEOS: HCl: H₂O = 1:59:348:2417). The mixed solution continued stirring for 24 h at 40°C. The gel obtained by the above stated was transferred into an autoclave with Teflon substrate, and then in the oven at 100°C crystallization was made for 48 h. The product was filtered, washed with deionized water, dried at room temperature. The white powder obtained was placed in a porcelain crucible and calcined for 24 h in a muffle furnace at 550°C to remove tri-block copolymer template. SBA-15 molecular sieve white powder was obtained [30].

2.3 Preparation of nano Ag₂S

380 mg of thiourea was weighed and placed into a 100 mL volumetric flask. Distilled water was added to prepare 0.05 mol/L thiourea aqueous solution. Three portions of 0.05 mol/L thiourea solutions prepared well were taken out, each was 20 mL.

17 mg of AgNO₃, 61 mg of sodium oleate and 20 mL of toluene were added into a conical flask, magnetically stirred and heated to 110°C. From the upper mouth of condenser pipe, 20 mL of the thiourea aqueous solution above-prepared was slowly added using 30 min.

After the reaction system was cooled to room temperature, there was an obvious interface layer between toluene phase and aqueous phase. The top was light black and the bottom was colorless solution. The two phases were separated by separating funnel and the upper toluene phase was retained. With high-speed centrifuge the centrifugal separation of toluene phase was carried out, and the precipitate obtained was dried to obtain the powder sample of Ag₂S nanoparticles according to the above-stated procedure [29].

2.4 Preparation of (SBA - 15) - Ag₂S nanocomposites

0.1000 g SBA-15 and 0.0010 g Ag₂S were weighed, the two samples were ground, sieved as powder, mixed well and placed into a muffle furnace at 500°C for thermal diffusion for 48 h. Then, the sample was cooled to room temperature, so as to obtain the (SBA-15)-Ag₂S nanocomposite with 1% Ag₂S (in weight). Using the same method, (SBA-15)-Ag₂S nanocomposites with 5%, 10%, 15% Ag₂S (in weight) were prepared. The percentage composition of composite materials is shown as Table 1.

Table 1
Composition of the composite material

Sample SBA-15(g) Ag₂S(g) Ag (g) S (g) Percentage of Ag₂S (w/w)

(1) 0.1000 0.0010 0.00087 0.00013 1%

(2) 0.1000 0.0053 0.00461 0.00069 5%

(3) 0.1000 0.0111 0.00966 0.00144 10%

(4) 0.1000 0.0176 0.01541 0.00229 15%

Sample	SBA-15(g)	Ag₂S(g)	Ag (g)	S (g)	Percentage of Ag₂S (w/w)
(1)	0.1000	0.0010	0.00087	0.00013	1%
(2)	0.1000	0.0053	0.00461	0.00069	5%
(3)	0.1000	0.0111	0.00966	0.00144	10%
(4)	0.1000	0.0176	0.01541	0.00229	15%

(1), (2), (3), (4) are (SBA-15)-Ag₂S nanocomposites with Ag₂S contents of 1%, 5%, 10% and 15% in weight, respectively.

2.5 Instrument and characterization technology

Information on crystal structure and characteristic of periodic arrangement were determined using D5005 X- ray diffractometer (German Siemens), Cu-K_α target, λ= 1.540560Å. Operating voltage (tube voltage) was 50 kV, the operating current was 150 mA with a scanning range of 0∼10° and a scanning step size of 0.02°. Over the scanning range of 10∼80°, the scanning step size was 0.2°. TEM experiments were carried out on a instrument (Japanese Electronics Corporation) JEM-2010 equipment. Point resolution was 0.19 nm and the operation voltage was 120 kV. Low temperature nitrogen adsorption-desorption was measured at 77 K under liquid nitrogen condition on ASAP 2020 V3.01 H type adsorption analyzer of American Micromeritics Company. The samples were activated at 363 K by vacuum pumping for 12 h. Data were calculated by Bdb (Broekhoff and de Boer) method [31], the specific surface was determined according to BET (Brunner-Emmett-Teller) method [32], and BJH (Barrett-Joyner-Halenda) method was used to analyze the pore size distribution [33]. FT-IR spectrometer, the instrument used was VERTEX70 type produced in German Brook Company. KBr tablet technology was used. The number of scans was selected to be 32 time. The scanning range was 400–4000 cm^–1 with a resolution of 4 cm^–1. Luminescence experiment was carried out on a Japanese Hitachi U-4100 type equipment, the working environment of the instrument was 25±1°C. Ultraviolet-visible diffuse reflectance spectra were determined on a Japanese Hitachi F-7000 instrument. The operating environment of the instrument was 25±1°C with α-Al₂O₃ as matrix.

3 Results and discussion

3.1 Chemical analysis

Ag content was determined by spectrophotometry [34]. The content of S was measured by weight method. Ag and S contents were obtained in the nano composite materials, respectively. Thus, the percentage of Ag₂S in the nanocomposite was obtained. The analytical results showed that the percentage of Ag₂S in the composites is the same as those of the added Ag₂S in the composite materials, the calculated results are shown in Table 1.

3.2 XRD characterization of samples

Figure 1 shows small angle XRD patterns of host SBA-15 and different Ag₂S percentage nanocomposites. It can be seen from the curve (a) that the SBA-15 prepared has three diffraction peaks, respectively, which can be assigned to the diffraction peaks obtained by (100), (110) and (200) crystal plane diffraction. The diffraction peak positions are consistent with those reported in literatures [19, 30], proving that the material synthesized was SBA-15. By comparing the different percentages Ag₂S composite materials and SBA-15 in Fig. 1, it can be found that diffraction intensity of the composites with different percentage of Ag₂S has some difference. With the increase of Ag₂S content in the composites, the 2θ values of their diffraction peaks decreased gradually. Migration of diffraction peaks indicates that Ag₂S went into the molecular sieves, thereby leading to migration of the diffraction peak and decrease in intensity of diffraction peak, but the characteristic peaks of SBA-15 did not disappear. This shows that after the diffusion of Ag₂S into SBA-15 the SBA-15 architecture framework was not damaged.

Fig.1

Small angle XRD patterns of host SBA-15, guest Ag₂S and nanocomposites with different content of Ag₂S: (a) SBA-15, (b) (SBA-15)-(1%)Ag₂S nanocomposite, (c) (SBA-15)-(5%)Ag₂S nanocomposite, (d) (SBA-15)-(10%)Ag₂S nanocomposites, (e) (SBA-15)-(15%)Ag₂S nanocomposite, (f) Ag₂S.

Figure 2 shows wide angle XRD patterns of the guest Ag₂S and the Ag₂S nanocomposites with different percentage. The size of nano silver sulfide can be calculated by Scherrer formula using the pattern of nano silver sulfide (curve a) in the figure. The Scherrer formula is as follows:

Fig.2

Wide-angle XRD patterns of guest Ag₂S and nanocomposites with different content of Ag₂S: (a) Ag₂S, (b) (SBA-15)-(1%)Ag₂S nanocomposite, (c) (SBA-15)-(5%)Ag₂S nanocomposite, (d) (SBA-15)-(10%)Ag₂S nanocomposite, (e) (SBA-15)-(15%)Ag₂S nanocomposite.

$d = K λ / (β cos θ)$ (1)

In the formula, d-grain size along the direction perpendicular to the {h, k, l} crystal plane (nm). K - Scherrer constant,λ- X-ray wavelength, θ- Bragg angle, deg, β- the main peak FWHM corresponds to the radian value, rad.

According to calculation of the Scherrer formula, the dimension of Ag₂S obtained is d = 6.2 nm (K = 0.89, λ= 0.154 nm).

The dimension of (SBA-15)-Ag₂S (1, 5, 10, 15%) nanocomposite material is d = 4.50, 4.40, 3.62, 3.24 nm (K = 0.89,λ= 0.154 nm).

After the comparison of Ag₂S composite materials with different percentage with Ag₂S in Fig. 2, it is found that intensity of the diffraction peak has been obviously decreased. Especially, for 1% content composite material no diffraction peak of Ag₂S appeared, indicating that Ag₂S completely diffused into the SBA-15 molecular sieve. The peak values of the other composite materials also had certain decrease. With the increase of the content of Ag₂S, the characteristic peaks of Ag₂S in composite materials appeared. This indicated that when the content of Ag₂S is higher, it not only diffused into SBA-15 molecular sieve channels, but also at the same time gathered in the molecular sieve surface. The characteristic peaks of Ag₂S were detected. The diffusion effect of the composite material with smaller Ag₂S percentage is better. According to the Bragg equation d = nλ/(2sinθ), d₁₀₀ and a₀ parameters can be calculated and the calculated results are shown as Table 2.

Table 2

θ, d₁₀₀ and a₀ parameters of SBA-15 and composite materials with different content of Ag₂S

Material	2θ	d₁₀₀/(nm)	a₀/(nm)
SBA-15	0.92	9.5909	11.075
(SBA-15)-(1%)Ag₂S	0.84	10.504	12.129
(SBA-15)-(5%)Ag₂S	0.83	10.631	12.276
(SBA-15)-(10%)Ag₂S	0.82	10.643	12.297
(SBA-15)-(15%)Ag₂S	0.86	10.260	11.847

Note: n = 1, λ= 0.154 nm, $a_{0} = 2 d_{100} / \sqrt{3}$ .

3.3 Study on pore size distribution of samples

Figure 3(A) shows N₂ adsorption-desorption curve of SBA-15 as well as (SBA-15)-Ag₂S composites with different Ag₂S content at 77 K. It can be seen from the figure that the curves of the several composite materials belong to the Langmuir type IV isotherm and have the hysteresis loops of H1 type, which indicates that the composites still have the properties of mesoporous materials. The pore structure parameters of the samples are listed in Table 3. After Ag₂S was introduced into the SBA-15, the BET specific surface area of SBA-15 was reduced from 613 m²/g to 409 m²/g, pore volume was reduced from 0.99 cm³/g to 0.69 cm³/g, indicating that Ag₂S had been assembled into the SBA-15 channels. The thickness of pore wall was increased from 4.45 nm to 5.17 nm, which may be because a small amount of Ag₂S nano particles were adsorbed on the surfaces of SBA-15, resulting in an increase in the wall thickness. Figure 3 (B) is the pore size distribution patterns of SBA-15 and the (SBA-15)-Ag₂S composites with different Ag₂S content. By contrast, it can be known (Table 3) that the aperture of host in the (SBA-15)-Ag₂S nanocomposite decreased to some extent. This is because when Ag₂S went into the SBA-15, part of the Ag₂S migrated into the mesoporous molecular sieve pores and led to the aperture size to become smaller.

Fig.3

N₂ adsorption-desorption curves (A) and pore size distribution (B) of samples at low temperature: (a) SBA-15, (b) (SBA-15)-(1%)Ag₂S nanocomposite, (c) (SBA-15)-(5%)Ag₂S nanocomposite, (d) (SBA-15)-(10%)Ag₂S nanocomposite, (e) (SBA-15)-(15%)Ag₂S nanocomposite.

Table 3

Aperture structure parameters of samples

Sample	Interplanar distance d₁₀₀(nm)	Cell parameter a₀^a(nm)	BET specific surface area (m²/g)	Pore volume ^b(cm³/g)	Pore size ^c(nm)	Pore wall thickness ^d(nm)	Ag₂S content (%)
SBA-15	9.5909	11.075	613	0.99	6.63	4.45	0
(SBA-15)- (1%)Ag₂S	10.504	12.129	598	0.91	6.60	4.48	1.0
(SBA-15)- (5%)Ag₂S	10.631	12.276	501	0.87	6.37	4.78	5.0
(SBA-15)- (10%)Ag₂S	9.5909	11.075	465	0.80	6.12	4.92	10.0
(SBA-15)- (15%)Ag₂S	10.260	11.847	409	0.69	5.21	5.17	15.0

Note: (a) Cell parameter, $a_{0} = \frac{2}{\sqrt{3}} d_{100}$ ; (b) BJH adsorption cumulative pore volume; (c) Pore size calculated from the adsorption curve; (d) Cell parameters (a₀) – pore size (most probable aperture)=pore wall thickness.

3.4 Infrared spectroscopic characterization of samples

Figure 4 shows infrared spectra of host SBA-15, guest Ag₂S and nanocomposites, where curve a is infrared spectrum of nano Ag₂S, curve b is infrared spectrum of SBA-15, curves c, d, e, f, are the infrared spectra of (SBA-15)-Ag₂S nanocomposites with 1%, 5%, 10% and 15% Ag₂S, respectively. It can be seen from the curve a that there are absorption peaks at 494 cm^–1 and 737 cm^–1, which are the characteristic peaks of Ag₂S. In curve b, the characteristic absorption peak at 471 cm^–1 corresponds to the T-O bending vibration peak of Si-O-Si bond of SBA-15 skeleton, and the absorption peak at 820 cm^–1 is Si-O-Si symmetric stretching vibration peak corresponding to the SiO₄ tetrahedral of SBA-15 molecular sieve. The 1107 cm^–1 broad absorption peak is the asymmetric stretching peak of Si-O-Si, while the peak corresponding to the absorption at 1657 cm^–1 is the characteristic peak of -OH. In addition, the absorption peak at 2370 cm^–1 is the characteristic peak of CO₂. The absorption peak at 3470 cm^–1 is the characteristic peak of H₂O. Compared curve c, d, e, f with curve b, it can be seen that the infrared spectra of the (SBA-15)-Ag₂S nanocomposites after encapsulation of Ag₂S did not show characteristic peaks of Ag₂S, suggesting that the Ag₂S was maybe evenly dispersed in molecular sieve pores in the form of quantum dots.

Fig.4

Infrared spectra of host SBA-15, guest Ag₂S and nanocomposites: (a) Ag₂S, (b) SBA-15, (c) (SBA-15)-(1%)Ag₂S nanocomposite, (d) (SBA-15)-(5%)Ag₂S nanocomposite, (e) (SBA-15)-(10%)Ag₂S nanocomposite, (f) (SBA-15)-(15%)Ag₂S nanocomposite.

3.5 Transmission electron microscopic (TEM) characterization of the samples

Figure 5 (a) and (b) show the transmission electron micrograph of SBA-15 and (SBA-15)-Ag₂S nanocomposite with 10% Ag₂S, respectively. It can clearly be seen from the figure that the channels are obvious and are not destroyed. Compared with the TEM picture of SBA-15, although for the composite a slight agglomeration phenomenon appeared, the stability of channels was not affected and the channels were not destroyed.

Fig.5

TEM picture of (a) SBA-15 and (b) (SBA-15)-Ag₂S nanocomposite.

3.6 UV-Vis diffuse reflectance spectra of samples

Figure 6 shows the UV-Vis diffuse reflectance spectra of the samples. The curves a, b, c, d, e and f are the UV-Vis diffuse reflectance spectra of SBA-15, Ag₂S, (SBA-15)-Ag₂S(1%): (SBA-15)-Ag₂S(5%): (SBA-15)-Ag₂S(10%) and (SBA-15)-Ag₂S(15%), respectively. It is shown that the SBA-15 molecular sieve unencapsulated did not absorb UV-Vis light. After loading Ag₂S, (SBA-15)-Ag₂S nanocomposite produced an absorption. The UV-visible absorption peak of the composite is located at 246 nm, with a blue shift of 38 nm relative to the absorption peak of Ag₂S at 284 nm. The reason for the blue shift is that the energy of the forbidden band increases, which is caused by the steric confinement effect of channels of the SBA-15 molecular sieve. At the same time, it further explains that the Ag₂S was in the SBA-15 molecular sieve channels. Because SBA-15 has a huge surface area, it provides enough space for the embedded Ag₂S nano particles and provided enough space to enable the Ag₂S molecules to maintain a certain distance between each other, which makes Ag₂S easier in the form of monomer be adsorbed on the pore walls of mesoporous SBA-15. The results of the UV-Vis spectra further showed that the Ag₂S molecules were well assembled into SBA-15 channels and presented a highly dispersed state.

Fig.6

UV-Vis diffuse reflectance spectra of samples: (a) SBA -15, (b) Ag₂S, (c) (SBA-15)-(1%)Ag₂S nanocomposite, (d) (SBA-15)-(5%)Ag₂S nanocomposite, (e) (SBA-15)-(10%)Ag₂S nanocomposite, (f) (SBA-15)-(15%)Ag₂S nanocomposite.

3.7 Fluorescence spectra of samples

Figure 7 shows the fluorescence spectra of Ag₂S and nano composite materials. The wavelength 200–400 nm corresponds to the excitation spectrum, the wavelength 400–700 nm corresponds to the emission spectrum. The curve a is the fluorescence spectrum of nano Ag₂S, and the curves b, c, d, e are fluorescence spectra of the (SBA-15)-Ag₂S nanocomposites incorporated 1%, 5%, 10% and 15% of Ag₂S, respectively. Photoluminescence spectrum of semiconductor nanocrystal generally includes two luminescence bands: one is narrow and weak luminescent peak located at the ultraviolet area, which is caused by the transitions between the energy levels of excitons whose band edge is discrete. It is called band edge or exciton emission. The other one is wide and strong luminescence band is located in the visible light region. It is generally considered the transition caused by impurities or defects, called impurity or defect emission. In this study, the peak position of the emission spectrum appeared at 425 nm, which is in the visible range. Because the size of the Ag₂S in the sample is small, the probability of forming defects on the surface of the nanoparticles is high. Therefore, the luminescence in this study should be caused by surface defects. SBA-15 itself does not have the luminescent properties, but after the assembly of Ag₂S the composite material presented luminescence and compared with Ag₂S itself the luminescent intensity increased obviously, indicating that after the assembly of Ag₂S in the molecular sieve SBA-15 the luminescence ability increased compared with Ag₂S. The (SBA-15)-Ag₂S has a potential application prospect as a light emitting diode etc optical materials.

Fig.7

Luminescence spectra of Ag₂S and nanocomposite material: (a) Ag₂S, (b) (SBA-15)-(1%)Ag₂S nanocomposite, (c) (SBA-15)-(5%)Ag₂S nanocomposite, (d) (SBA-15)- (10%)Ag₂S nanocomposite, (e) (SBA-15)-(15%)Ag₂S nanocomposite.

4 Conclusions

In this paper, (SBA-15)-Ag₂S host-guest nanocomposites were prepared. The assembled silver sulfide did not destroy the molecular sieve skeleton and the prepared host-guest nanocomposite still maintained good crystallinity. The guest has already partly occupied the molecular sieve pores. UV-Vis reflectance absorption spectra showed that Ag₂S molecules were well assembled into SBA-15 and highly dispersed. The (SBA-15)-Ag₂S nanocomposites have luminescent phenomena and the luminescence is stronger than that of Ag₂S. The (SBA-15)-Ag₂S nanocomposites have obvious luminescence at 425 nm, which has a potential applied prospect as a light emitting diode etc optical materials.

Footnotes

Acknowledgments

This study was funded by the Natural Science Foundation of Jilin Provincial Science and Technology Department from the Science and Technology Development Program of Jilin Province, China. The project number was 20180101180JC, 222180102051, KYC-JC-XM-2018-051. The authors express their thanks.

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Preparation,characterization and luminescence of (SBA-15)-Ag 2 S nanocomposite material

Abstract

Keywords

1 Introduction

2 Experimental

2.1 Reagent and instrument

2.2 Synthesis of SBA-15 molecular sieve

2.3 Preparation of nano Ag2S

2.4 Preparation of (SBA - 15) - Ag2S nanocomposites

Table 1 Composition of the composite material Sample SBA-15(g) Ag2S(g) Ag (g) S (g) Percentage of Ag2S (w/w) (1) 0.1000 0.0010 0.00087 0.00013 1% (2) 0.1000 0.0053 0.00461 0.00069 5% (3) 0.1000 0.0111 0.00966 0.00144 10% (4) 0.1000 0.0176 0.01541 0.00229 15%

3 Results and discussion

3.1 Chemical analysis

3.2 XRD characterization of samples

Footnotes

Acknowledgments

References

2.3 Preparation of nano Ag₂S

2.4 Preparation of (SBA - 15) - Ag₂S nanocomposites

Table 1
Composition of the composite material

Sample SBA-15(g) Ag₂S(g) Ag (g) S (g) Percentage of Ag₂S (w/w)

(1) 0.1000 0.0010 0.00087 0.00013 1%

(2) 0.1000 0.0053 0.00461 0.00069 5%

(3) 0.1000 0.0111 0.00966 0.00144 10%

(4) 0.1000 0.0176 0.01541 0.00229 15%