Sensor for obtaining giant raman scattering spectra and method of making said sensor

FIELD: chemistry.

SUBSTANCE: invention relates to a method of making a sensor for obtaining giant Raman scattering spectra, which is a glass capillary whose inner wall is coated with silver nanoparticles. The silver nanoparticles are obtained and attached to the glass surface via reduction of silver ions with alkylamines. The glass capillaries are washed with a detergent solution for optical devices, distilled water while mixing with ultrasound, absolute ethanol and dried in air, placed in a teflon vessel with a reaction mixture of 1 mmol/l AgNO3 and 1 mmol/l alkylamine in ethanol; the reaction mixture is heated at 45-50°C for 40 min with intense agitation along the axis of the capillaries. After the reduction reaction, the capillaries are washed with ethanol and cleaned on the outside.

EFFECT: invention enables to obtain a high-resolution giant Raman scattering sensor.

2 cl, 4 ex


The invention relates to nanotechnology. In particular, to obtain sensors for identifying and determining the concentrations of various substances using the spectra of giant Raman scattering.

- Enhanced Raman scattering (GOR) is an effect, the essence of which is to substantially increase the intensity of the Raman signal of adsorbed molecules when adsorbed on metal surfaces, when the adsorbed molecules may have an abnormally high value of the cross section of Raman scattering of light due to electron transfer from the surface of metal nanoparticles on the molecule.

Existing sensors receive a coating of metal (silver, gold) on the basis of, for example, made of silicon probe. Article: Nanoscale chemical analysis by tip-enhanced Raman spectroscopy, Raoul M. Stockle, Yung Doug Suh, Volker Deckert 1, Renato Zenobi, Chemical Physics Letters 318, 2000, 131-136, a probe for an atomic force microscope, made of silicon, deposited silver. In the article "a Simple Chemical Method for Forming Silver Surfaces with Controlled Grain Sizes for Surface Plasmon Experiments" Y. Saito, J. J. Wang, D. N. Batchelder, and D. A. Smith, - Langmuir 2003, 19, 6857-6861 is disclosed a method of manufacturing a sensor by chemical deposition of silver (the silver mirror reaction) on a flat basis. The coating on the base has the disadvantage of creating a nonuniform layer of silver nanoparticles. Chemical osuzhdeni is through reaction of the silver mirror is complicated by the influence of carbon dioxide of the atmosphere at the complex of silver ion with ammonia. Note that even the breath of the experimenter can affect the reaction of the silver mirror.

Closest to the proposed sensor is a known sensor for obtaining spectra of GOR, which is a glass capillary tube, on the inner side of which is coated with silver nanoparticles (see WO 2008116093 A2, 25.09. 2008, prototype)

In the known sensor silver nanoparticles on the substrate surface are in the composition and therefore the dimensional effect GOR to identify and determine the concentration of substances weakened.

The task of the invention to provide using the proposed sensors spectra GOR with high resolution.

The problem is solved by a method of manufacturing a sensor for obtaining spectra of GOR, which is a glass capillary tube, on the inner side of which is coated with silver nanoparticles produced according to the invention, the attachment to the glass surface of silver nanoparticles through reduction reaction of silver ions bonds alkylamines. The method according to the invention, is carried out in the following sequence.

Take a glass capillary, preferably with capillary effect of raising solution for convenient analysis. With an inner diameter slightly larger diameter of the needle of the syringe to be placed in the capillary researched solution. The capillary was washed with detergent is redstem for optics, distilled water, ethanol. Dried in air at 70°C for 30-40 minutes and Then the capillary is placed in a Teflon beaker with a reaction mixture of 1 mmol/l AgNO3and 1 mmol/l of the alkylamine in ethanol. The reaction mixture is heated at 70°C for 30-40 minutes, Preferably under stirring along the axis of the capillary. After the reduction reaction of the capillary is washed with ethanol and purified from the outside.

The inside glass capillaries as the basis convenient for several reasons. First, the reaction occurring therein, is separated from the atmosphere. Secondly, after applying a layer of silver nanoparticles and receiving sensor analyzed the solution can be entered by dipping the tip of the capillary in the analyzed solution, which will spontaneously enter into the capillary by capillary forces. If this method does not allow you to enter an analyte in the capillary, it is injected with a syringe. Thirdly, the capillaries can be stored for long periods, covering them from the atmosphere plastic and inert to silver substance, such as paraffin. The reaction must be carried out in a Teflon beaker from wasting reagents in the case of reaction in a glass vessel, which is covered with a layer of silver nanoparticles. During the reaction layer of the nanoparticles, not only covered the inside of the capillary, but also external. Therefore, is and must be cleaned from the layer of silver nanoparticles. In the reaction used primary amines: butylamine, ethanolamine. The invention is illustrated in the examples.

The method of producing the sensor. Example 1. To obtain the sensor take a glass capillary with an inner diameter of 0.9 mm, a wall thickness of 0.3 mm and length 10 mm Capillary together with other capillaries are washed with 0.5% detergent solution for optics Helmanex II at pH=9.5 for 3 hours, and then distilled water (resistivity greater than 18 Mω·cm) under stirring ultrasound. Then washed with absolute ethanol and dried in air at 70°C for 30-40 minutes and Then the capillary is placed in a Teflon beaker with a reaction mixture of 1 mmol/l AgNO3and 1 mmol/l of butylamine in ethanol. The reaction mixture was heated at 45-50°C for 40 min under vigorous stirring along the axis of the capillary. After the reduction reaction of the capillary is washed with ethanol and purified wool on the outside. Air-dried. Get the sensor in the form of a glass capillary on the inner side of which is attached silver nanoparticles of size 92±35 nm.

The method of producing the sensor. Example 2. Sensor gain as in example 1, except that instead of butylamine take ethanolamine. Get the sensor size of the nanoparticles 102±35 nm.

Obtaining the spectrum of GOR. Example 1. Prepare a 2.5·10-5M solution bestiola in methanol. To the surface of the solution touch the end of the Senso is and. The solution will rise to 3 mm in inner channel of the sensor. The methanol from the sensor is removed by drying in air. Then get range on GOR combined system OmegaScope™, combining scanning probe microscope with confocal Raman and fluorescence spectrometer company Aist NT. Use a blue laser with a wavelength of 473 nm, an average power of 25 mW and a laser spot with a diameter of 500 nm. The exposure time 30 s Receive a range of GOR, in which analysis to choose the band 1573 cm-1. Determine its intensity and pre-constructed calibration curve to determine the concentration bestiola 2.4 x 10-5M

Obtaining the spectrum of GOR. Example 2. Cook 5·10-6M solution of adenine in distilled water. Prepare the sample to obtain a spectrum GOR, as in example 1. Shooting range during exposure to 2 C. For analysis, you can select the band with the maximum scattering at 734 cm-1. Determine its intensity and pre-constructed calibration curve the concentration of adenine 5.2 x 10-6M

Thus, the proposed sensor suitable for storage, allows to obtain spectra of GOR with a small content of substances in solutions and therefore can be applied in practice.

1. A method of manufacturing a sensor for obtaining spectra of GOR, which is a glass capillary, vnutrenniy the side of which is coated with silver nanoparticles, characterized in that the silver nanoparticles are obtained and attached to a glass surface using a reduction reaction of silver ions bonds alkylamines, namely the glass capillary is washed with wash solution for optics, distilled water with stirring, ultrasound, absolute ethanol and air-dried, placed in a Teflon beaker with a reaction mixture of 1 mmol/l AgNO3and 1 mmol/l of the alkylamine in ethanol, the reaction mixture is heated at 45-50°C for 40 min under vigorous stirring along the axis of the capillary, after the reduction reaction of the capillary is washed with ethanol and purified from the outside.

2. The method according to p. 1, characterized in that the recovery of silver ions using butylamine and ethanolamine.


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