Method of obtaining semiconductor colloidal silver sulfide quantum dots

FIELD: chemistry.

SUBSTANCE: invention relates to colloidal chemistry and can be used in luminescent labels, as well as in production of materials for lasers, light diodes, solar panels, and photocatalysts. First, sodium sulfide and silver nitrate are prepared separately. For this purpose 0.01-0.5 g of sodium sulfide and 0.01-0.5 silver nitrate are dissolved in 40-200 ml of cold distilled water. 0.5-20 g of gelatin swell in reactor for 30 min in 100-500 ml of distilled water with temperature from 20-30°C. Obtained gelatin solution is heated to 40-90°C with mixing, 5 ml of 96% ethanol are poured into it. After that, double-stream pouring of prepared solutions of sodium sulfide and silver nitrate is realised, with further heating for 10-20 min with obtaining sol of colloidal silver sulfide quantum dots and cooling to 4-10°C for 10 hours. Obtained jelly is crushed to size of granules 5-10 mm, washed with distilled water at temperature 7-13°C, excess of water is decanted and granules are heated to temperature higher than 40°C.

EFFECT: invention makes it possible to obtain silver sulfide quantum dots with size 1-5 nm in gelatin matrix, luminescent in the range 800-1100 nm.

2 cl, 4 dwg, 2 ex

 

The invention relates to colloidal chemistry, namely the production of semiconductor colloidal quantum dots Ag2S in a dielectric matrix.

Quantum dots Ag2S can be used as fluorescent labels, as well as material for lasers, LEDs and solar cells. In addition, they are of great interest from the point of view of photocatalysis, photovoltaics, biomedical applications, etc. due to the low toxicity of sulphide of silver and a small width of the forbidden band of quantum dots Ag2S.

A method of obtaining quantum dots Ag2S, dispersed in the polyacrylamide (J.-F. Zhu et al., J. Phys. Chem. C, 2007, 111, 3920-3926). Obtaining quantum dots by using microwave heating of ethylene glycol containing AgNO3, sulfur and acrylamide at a temperature of ~125°C. resulting In the formation of nanoparticles Ag2S and polymerization of acrylamide, the resulting nanoparticles of silver sulfide, which are evenly distributed in the matrix of polyacrylamide. The size of the resulting particles 36-54 nm, the average diameter 43.8 nm.

The disadvantages of this method of synthesis are: large size, long duration of synthesis (about 60 min), in addition, there is no evidence of conjugation with biologically active molecules.

A method of obtaining the call is innych quantum dots Ag 2S (Yaping Du et al., J. Am. Chem. Soc.,2010.V. 132, No. 5, 1470-1471) using Ag(DDTC) as a precursor. Its aqueous solution, oleic acid, octadecylamine and octadecan was heated to 100°C in one tank to remove water and oxides. As a result, formed a homogeneous brown solution. Then the mixture was heated up to 200°C in an atmosphere of N2and was maintained for 30 minutes. After which it was cooled, stirred and dried in air at 60°C. the Size of the resultant nanoparticles were 10.2 nm.

The main disadvantages of this method are the complexity and intensity of the process, the toxicity of the fusion components (octadecylamine), as a consequence, the lack of biocompatibility, as well as the lack of data on the conjugation with biologically active molecules.

Also in the literature (Q. Tang et al., Langmuir, 2006. Vol.22, 2802-2805) a description of the method of synthesis of quantum dots Ag2S using high-temperature injection single-component precursor Ag(SCOPh) dissolved in though. The synthesis was carried out as follows: degassed precursor (monitorenter silver) injectively in a special flask containing the room though a certain temperature in nitrogen atmosphere, then the temperature was increased at a rate of 1°C/sec. Upon reaching 160°C increase in temperature stayed with the ect was maintained for 10 minutes. The size of the resulting quantum dots was 20-30 nm.

A significant disadvantage of this synthesis is the high toxicity of the used solvent - though, careful empirical approach to the development of conditions of control of the synthesis parameters (initial temperature of the mixture, the heating rate, degassing precursor), lack of biocompatibility, lack of data about the possibility of pairing with biologically active molecules.

A method of obtaining self-organized periodic structures of nanocrystals in micellar solutions of surface-active substances (surfactants) patent RU 2317941 (IPC B82B 3/00, from 27.02.2008), which is to obtain nanoparticles of silver sulfide, using the exchange reaction between microemulsions of silver nitrate and sodium sulfide in isooctane, followed by addition of s-dodecylamine chloride (DTH) as extragent. This method allows to obtain nanoparticles Ag2S with an average size of ~5 nm.

The disadvantages of this method are the use of highly toxic compounds DTH, complexity, lack of biocompatibility of the obtained nanoparticles due to the presence of toxic components of the synthesis, the lack of data on the conjugation with biologically active molecules.

The prototype of the present invention is the method according to patent RU 2292573 (IPC G03C 1/2 from 27.01.2007), lets get submergibility silver halide photographic emulsion with an average size of microcrystals of silver halide 5-10 nm, which is a single emulsification with an excess of silver ions is the introduction of an aqueous solution of bromide and potassium iodide in an aqueous solution of silver nitrate and gelatin in 1-2 minutes with vigorous stirring, the concentration by freezing with subsequent washing. Stage emulsification and maturation combined in this method of synthesis.

This method allows you to obtain crystals of AgBr, but because they have a high sensitivity, due to which photodissociate, this creates difficulties in storage and use. The crystals of silver bromide does not have the ability to luminescence.

The objective of the invention is to develop a method for the synthesis of nanocrystals of silver sulfide capable of conjugation with biologically active molecules, without the use of toxic compounds

The technical result of the present invention is in the low-temperature synthesis of the Sol-gel method nanocrystals of silver sulfide in size from 1 to 5 nm in a polymer matrix with luminescence in the field of 800-1100 nm.

The technical result is achieved in that in the method of obtaining the floor is provodnikov colloidal quantum dots of silver sulfide, including doctrine merging into the reactor solutions of the reagent and of silver nitrate, heating and mixing with gelatin, cooling, washing, according to the invention as a solution of the reagent used is 0.01-0.5 g of sodium sulfide in 40-200 ml of cold distilled water, a solution of silver nitrate comprises from 0.01 to 0.5 g of the substance and 40-200 ml of cold distilled water until the draining of the reagent solutions of silver nitrate and 0.5 to 20 g of gelatin swells in the reactor for 30 min in 100-500 ml of distilled water temperatures ranging from 20 to 30°C, then, a gelatin solution with stirring is heated to 40-90°C and it blends in 5 ml of 96% ethanol and then the solution of the reagent and nitrate of silver; mixing at a given temperature continue 10-20 min; cooling is to a temperature of from 4 to 10°C, at which the solution is aged for 10 hours, after which the frozen solution is crushed to grain size of 5-10 mm, the washing is conducted with distilled water at a temperature of from 7 to 13°C, then the excess water is decanted, the pellets are heated to a temperature above 40°C.

As a stabilizer in gelatin add STA-Sol in an amount of from 0.1 to 4% of the mass. gelatine.

In Fig.1 shows (a) an electronic photograph CT Ag2S and (b) histogram of the distribution of the size of the CT Ag2S, dispersed in VC the tin without the use of additional stabilizers.

In Fig.2 shows the diffraction pattern dispersed in gelatin colloidal CT Ag2S.

In Fig.3 shows absorption spectra of (a) ensembles of colloidal CT Ag2S of various sizes and associates "CT Ag2S - methylene blue", and (b) CT Ag2S in the presence of a hundred-salt.

In Fig.4 shows the spectra of the luminescence of colloidal CT Ag2S, (a) pure and (b) in the presence of a hundred-salt.

Example 1

The reactor is filled with 300 ml of cold distilled water 25±5°C and loaded with 7.5 g of gelatin, which is within 30 minutes swells. Next, the reactor was placed a stir bar, connected to the motor and to the power supply of the motor, mercury thermometer and the electrodes connected to the pH meter.

Then 0.262 g of silver nitrate dissolved in 100 ml of cold distilled water and 0.18 g of sodium sulfide in 100 ml of cold distilled water 25±5°C in glass jars. Silicone tubing connected to a peristaltic pump and immersed in beakers with solutions of silver nitrate and sodium sulfide, and then include a pump to remove air from silicone tubing. Further included a liquid thermostat for heating the reactor to a predetermined temperature of 70°C and the mixer is turned on, the speed of rotation of which about 200 rpm When reaching into the reactor to the desired temperature, which is controlled by a mercury thermometer in the reactor shown is W 5 ml of ethanol 96% to prevent foaming in the mixing gelatin solution, then the reactor is placed silicone tubing connected to a peristaltic pump and glasses with solutions of silver nitrate and sodium sulfide. Included peristaltic pump. Merging the solutions of salts enter into a chemical reaction, the result of which is the formation of quantum dots of silver sulfide. After the salt solutions of silver nitrate and sodium sulfide is completely merged into the reactor, turn off the peristaltic pump and stirring for 10 min to achieve maximum uniformity in the size of the resulting colloidal quantum dots. Upon completion of mixing the prepared Sol of colloidal quantum dots is poured in a glass beaker and placed in a refrigerator at a temperature of 7±3°C for a period of approximately 10 hours for hardening gelatin solution. After this time a gelatin gel containing quantum dots of silver sulfide, is crushed to the size of the granules from 5 to 10 mm and loaded into 5 liters of cold distilled water 10±3°C for 30 minutes to remove soluble products of a chemical reaction. After the granules of gelatin gel containing colloidal quantum dots of silver sulfide, throw on a gauze to remove excess water and leave to drain for 30 minutes. Next gelatin granules are loaded into the article the glass beaker and melted by heating up to T≥40°C.

E-pictures and the histogram of the size distribution of colloidal CT Ag2S (Fig.1) shows that the methodology allows to obtain CT Ag2S in the gelatin, the amount of which does not exceed 5 nm, which is 3 times higher than the Bohr radius of an exciton in a massive crystal Ag2S (1.5 nm). The results of measurements carried out using transmission electron microscopy showed that synthesized by the method described above CT Ag2S in the gelatinous matrix are isolated an average diameter of about 2.5 nm with a dispersion of about 30%. Obtained in this way colloidal quantum dots have a luminescence maximum 925 nm.

The methodology used allows conjugation of quantum dots Ag2S with molecules of biologically active substances (amino acids, dyes and other) upon completion of the synthesis. Conjugation of quantum dots of silver sulfide molecules of methylene blue (MG) produced by the introduction into the melt gelatin containing CT Ag2S, dye concentrations of 10-1and 10-2molar fractions to mixing.

Obtaining gelatin films is carried out by applying a gelatin solution containing colloidal quantum dots Ag2S, after heating and mixing of the glass plate-the base number from 1 to 10 ml per 20 cm2 of the glass plate, drying at a temperature of from 20 to 80°C for 2-24 hours.

Example 2

The synthesis of quantum dots Ag2S using a hundred-salt (4-hydroxy-6-methyl-1,3 .3m a,7-tetraethylene) as an additional stabilizer was carried out similarly to the method of example 1, but with the gelatin into the reactor was introduced stabilizer (STA-salt) in an amount of 0.02,

X-ray diffraction (Fig.2) CT scan obtained as described in example 1 by the way, was investigated on the diffractometer ARL X TRA (Switzerland) for Kα1copper. The sample, representing the filling of the nanocrystals sulphide of silver, was placed on a substrate made of crystalline quartz. Reflexes correspond to the planes of the monoclinic crystal lattice. The analysis shows that the resulting distribution of peak clearly corresponds to the monoclinic modification of sulphide of silver. All reflexes are broadened, which indicates that the manifestation of the quantum size effect. For a cubic crystal modification Ag2S characterized by the most intensive reflexes 25.9051°, 36.9617°, 45.6886°, which does not correspond to our distributions, in which the highest intensity peaks have 28.87°, 31.3611°, 34.4664°, 36.6492°, 37.7673° and 43.2531°.

Absorption spectra of the samples CT Ag1S (Fig.3) obtained immediately after synthesis (curve 1) in example 1 and after keeping for 3 hours at 90°C (curve 2), and the obtained spectra is ture absorption associates "CT Ag 2S - methylene blue with a concentration of 10-1mol. D. (curve 3) and 10-1mol. D. (curve 4). For the synthesized colloidal CT values of the effective width of the forbidden band of all considered samples significantly exceeded the width of the forbidden zone of the single crystal Ag2S, which is 0.9 eV, which corresponds to the manifestation of the quantum size effect.

CT obtained in the absence of biologically active molecules at a speed of Zola at a temperature of 90°C for 3 hours, there is a clear maximum in the region of 2.9 eV (curve 2). This maximum corresponds to the absorption in the region of the first most probable optical transition. For CT, not subjected to prolonged exposure at high temperature, a clear peak is not observed (curve 1). Moreover, it is difficult to select the feature in the spectrum, which is associated with a wide range of CT in size. For such ensembles CT absorption spectrum represents the sum of the absorption spectra of CT of different sizes. The data obtained indicate that in the absorption spectra obtained by this method CT Ag2S, is a manifestation of the quantum size effect, the consequence of which is the increase of the values of the effective width of the forbidden zone of nanocrystals. When pairing with BAM (methylene blue) in the absorption spectrum appear Maxi the minds in the region of 1.7-2.0 eV, characteristic absorption bands of the dye molecule.

Absorption spectra of CT Ag2S in the presence of a hundred-salt immediately after draining and 3 hours after draining represented by curves 5 and 6.

1. A method of obtaining a semiconductor colloidal quantum dots sulphide of silver, including the interaction of solutions of the starting reagents in the solution of gelatin, characterized in that the quality of reagents used is 0.01-0.5 g of sodium sulfide in 40-200 ml of cold distilled water and 0.01-0.5 g of silver nitrate in 40-200 ml of cold distilled water; 0.5 to 20 g of gelatin swells in the reactor for 30 min in 100-500 ml of distilled water temperatures ranging from 20 to 30°C, and then a gelatin solution with stirring is heated to 40-90°C and it blends in 5 ml of 96% ethanol, and implement doctrine merging solutions of sodium sulfide and silver nitrate, heating continue 10-20 min, the cooling occurs at a temperature of from 4 to 10°C for 10 hours, after which the resulting jelly is crushed to grain size of 5-10 mm, the washing is conducted with distilled water at a temperature of from 7 to 13°C, then the excess water is decanted and the pellets are heated to a temperature above 40°C.

2. The method according to p. 1, wherein adding to gelatin as a stabilizer hundred-salt from 0.1 to 4% of the mass. of gelatin.



 

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