Composition for making sensor coatings based on aqueous suspensions of nanoparticles and method of preparing composition

FIELD: chemistry.

SUBSTANCE: composition for making sensor coatings contains antimony-doped tin dioxide of the formula SbxSn1-xO2, where x=0.1-0.3, and water in ratio SbxSn1-xO2:H2O = 89-87:11-13 wt %. The method of preparing the composition involves hydrothermal treatment of tin and antimony hydroxides at 170C for 48 hours. The tin and antimony hydroxides are obtained by dissolving Sn and Sb metal in concentrated hydrochloric acid, 18-20 wt %, while adding 3-5 wt % concentrated HNO3. The obtained solution is 2-3 times diluted with distilled water and a calculated amount of ammonia solution is added. Using a simple scheme, the disclosed method enables to obtain nanoparticles of said composition SbxSn1-xO2 with size of 30 nm and surface area of 154 m2/g, which can be used as the basic component of electroconductive ink for printing sensor arrays and microcontacts.

EFFECT: low labour and power consumption.

3 cl, 6 dwg, 3 ex


The technical field to which the invention relates.

The invention relates to inorganic chemistry, in particular to a method for producing suspensions of nanoparticles of tin dioxide doped with antimony SbxSn1-xO2(x=0.1, 0.2, 0.3) for the production of touch conductive ink for inkjet microprinting.

The advantage of the material obtained is that the resulting suspension are electrically conductive ink, which when "soft" coating can form a nanostructured active coating on microcontact area, which leads to a larger area of the gas sorption of the analyte and therefore high sensitivity gas-printed sensors.

The level of technology

Today, inkjet printing nanosuspension plays an important role in the creation of various planar structures. An important feature in the formation of nanostructured coatings with the given topology is the creation of approaches for obtaining liquid colloidal solutions based on semiconductor particles. In most cases this problem is solved by the detection of one or more synthetic approaches used by different precursors and conditions of the synthesis.

In the patent (CN 101209856 Yuhan Lin; Li Haidong; Nana Zhao; Mao Jun; Yandi Fan; Xiangling Ji Method for synthesizing tin oxide nanocrystalline by mould plate method combined wth hydrothermal condition) is considered a method of obtaining nanocrystalline SnO 2by combining the template technique with hydrothermal treatment. By varying the synthesis conditions can be obtained nanoparticles of various shapes (spheres, ribbons) and size.

Conductive SnO2high sensitivity is obtained by doping tin hydroxide of the metals Pd, Pt, Au, followed by hydrothermal treatment of the mixture, drying the resulting product and annealing (JP2008020411 Jun Tamaoki; Matsushiro Masaru, Manufacturing method for tin oxide gas sensor and a tin oxide gas sensor). Unfortunately, obtaining such composites based on SnO2and precious metals requires quite a long step-by-step syntheses. Ink for inkjet printing of transparent conductive films based on SnO2containing aqueous alkaline solution of stannic acid, in the patent (JP2005015608 Uchida Takashi; Sato, Hajime, Inkjet ink for forming transparent conductive tin oxide film), is obtained by dissolving tin acid in alkaline solution, followed by adding a water-soluble polymer. The difference of the patent from the proposed development is in a completely different way to obtain water-soluble ink and alloying of tin dioxide antimony to improve conductivity. Izvesteni methods of obtaining tin oxide doped with antimony by hydrothermal treatment of the hydroxides of tin and antimony (JP 62223019 Nishikura Hiroshi; Yamamoto, Shin; Yukio Terao, Crystalline tin-antimony oxide sol and production threof) or by annealing slurry containing compounds of tin and antimony (US4775412 Nishikura Hiroshi; Yamamoto, Shin; Yukio Terao Aqueous sol of crystalline tin oxide solid solution containing antimony, and production thereof), but they do not provide further possibility of their use as an ink for inkjet microprinting.

The technical result

At low labor and energy costs and simple technical execution of the obtained nanoparticles of tin dioxide doped with antimony composition SbxSn1-xO2(x=0.1, 0.2, 0.3) with a size of ~ 30 nm and a surface area of 154 m2/g, which makes them promising for use, as a main component in sensory and conductive inks for inkjet microprinting.

Summary of the invention the task was solved by the present invention. Composition for receiving a touch coatings based on aqueous suspensions of nanoparticles with a size of 30 nm SnO2according to the invention contains tin dioxide doped with antimony composition SbxSn1-xO2(x=0.1-0.3) and water with a ratio SbxSn1-xO2:H2O (89-87:11-13 wt.%). This goal is achieved by a different invention. The method of obtaining these compositions, including hydrothermal processing of hydroxides of tin and antimony at a temperature of 170C for 48 hours.

The hydroxides of tin and antimony can be obtained by dissolving metallic Sn and Sb in concentrated hydrochloric acid (18-20 wt.%) with the addition of (-5 mass %) conc. HNO3and the resulting solution was diluted with distilled water 2-3 times and poured the calculated amount of ammonia solution.

Detailed description of the method of obtaining

Nanoparticles of tin dioxide doped with antimony composition SbxSn1-xO2where x=0.1-0.3, synthesized by hydrothermal treatment soosazhdennykh hydrated oxides of tin and antimony. Hydrothermal treatment was made as follows: Zadok was transferred into a Teflon vessel, placed in a steel autoclave, and was filled with water at about 80% volume. The autoclave was kept at 170C for 48 hours, cooled and then extracted the received gray-blue suspension.

To confirm physico-chemical properties of the resulting suspension was having it cryochemical drying in sublimator Labconco Freezone 6 at a pressure of ~20mbar, for which the original samples were diluted 10 times and was sprayed through a nozzle into liquid nitrogen. Frozen cryogeny tolerated in sublimator. Drying was continued for 2-3 days with a gradual increase in temperatures from -40C to +40C. the Annealing dried at room temperature samples xerogels were carried out in a tubular furnace (Nabertherm) in the temperature range of 300-700C for 10-15 hours.

Analysis of the phase composition of the samples SbxSn1-xO2(x=0.1, 0.2 and 0.3), obtained after cryochemical with is the loud and annealing at 700C for 15 hours, shows that they have the x-ray characteristic of the solid solutions with the structure of rutile, and do not contain appreciable quantities of impurities. (Fig.1). The increase in the degree of substitution of tin, antimony does not lead to significant changes of the lattice parameters, which is associated with an insignificant difference of ionic radii Sn4+and Sb5+in chetyrehmetrovaya environment.

The presence of alloying dioxide tin oxide, antimony confirmed by the characteristic blue - gray color of the suspension directly after the hydrothermal treatment, which is stored and after annealing.

The expected elemental composition of the xerogel was confirmed by the method of RSMA, in particular, to the total composition Sb0.1Sn0.9O2it can be estimated as Sb0.09(2)Sn0.94(5)O2.01(2)that clearly demonstrates an excellent match. Strongly broadened diffraction peaks of the solid solution is observed even in the initial samples received after cryochemical drying without additional annealing. This suggests that the formation of solid solution occurs already during hydrothermal processing.

A typical micrograph cryogenically dried suspension shown in Fig.2. Suspension there are two factions - ultrafine particles and their gel-like agglomerates. Existence is the existence of two fractions in suspension is also confirmed by dynamic light scattering. Figure 3 clearly shows the existence of two peaks in the distribution curve at ~30 nm and ~150 nm. The estimation of specific surface area, as one of the important factors that determine the dispersion of the obtained particles and the possibility of their practical use, gives a value of ~154 m2/g for sample Sb0.1Sn0.9O2". This value could be correlated with the detected microstructure characteristics and the distribution curve of the particle size.

The sensory properties of the xerogel was measured in the temperature range 100-200C with periodic introduction of 0.8 ppm NO2in a stream of inert carrier gas. The electrical conductivity of the obtained particles SbxSn1-xO2(x=0.1-0.3) were tested using a two-prong method. To this suspension was applied onto a glass substrate, dried in an oven at ~100C, and then tested the conductivity of the exposed film. The obtained samples had a resistance at the level of 10-100 Ohms when the distance between the measuring electrodes is ~1 mm and the film thickness of ~100-500 nm.

The invention is illustrated by the following drawings and examples.

1. The diffraction pattern of sample SbxSn1-xO2where x=0.1 after annealing at 700C

2. Data REM for cryogenically dried suspension SbxSn1-xO2where x=0.1, consisting of ultrafine particles and their gel-like agglomerates

3. The distribution of particle sizes for sample SbxSn1-xO2where x=0.2, obtained by the method of dynamic light scattering.

Fig.4. The results of measurements of the conductivity of the sample SbxSn1-xO2where x=0.1 at different temperatures in the presence of NO2in the gas atmosphere.

5. Curves weight loss for the samples SbxSn1-xO2x=0.1 and 0.3 (b).

Fig.6. Microstructure printed by the suspension of nanoparticles SbxSn1-xO2on a silicon substrate using a standard inkjet printer.

Example 1. The hydroxides of tin and antimony were obtained from chloride tin (IV) and antimony (V), which was synthesized by dissolving metallic Sn and Sb in conc. HCl (18 wt.%) with the addition of conc. HNO3(3 wt.%). To the resulting solution was diluted with water 2-3 times was added ammonia to neutralize. Formed a loose white precipitate hydroxides of tin and antimony repeatedly washed with distilled water until a negative reaction to Cl-and NH4+. The xerogel obtained by hydrothermal treatment of hydroxides, has a remarkable touch signal (Fig.4.) in relation to nitrogen oxides and reaches values of R0/Rg=30-40 at temperatures from 100 to 150C, where Ro- resistance in discomposure, Rgthe resistance in the atmosphere of NO2.

Example 2. The ink composition SbxSn1-xO2where x=0.1-0.3, obtained by hydrothermal treatment, characterized by the presence of water, after conducting a cryochemical drying according to the TGA mass loss occurs in two stages - first ends about 100C (~6 wt.% from the original sample), and the second lasts from 200C up to high temperatures (optional ~6 wt.%) (5A, b). The ink composition can be written as SbxSn1-xO2*H2Oh, where the ratio between SbxSn1-xO2:H2O be (89-87:11-13 wt.%).

Example 3.

Microprinting of planar structures on stainless steel and silicon substrate in the form of two parallel arrows thickness of about 200 nm (figure 6) was carried out using a standard inkjet printer (Epson) with a set of additional empty cartridges, which placed produced by the hydrothermal method of suspension SbxSn1-xO2, x=0.1-0.3.

The material proposed in the present invention, is of great interest for use as the main component of the electrically conductive ink for inkjet microprinting various objects by controlled distribution of micropore suspension, for example, to print touch matrices or point contacts.

1. Composition for obtaining touch the coatings based on aqueous suspensions of nanoparticles with a size of 30 nm tin dioxide, characterized in that it contains tin dioxide doped with antimony, composition SbxSn1-xO2where x=0.1 to 0.3, and water with a ratio SbxSn1-xO2:H2O equal 89-87: 11-13 wt.%.

2. A method of obtaining a composition according to claim 1, including hydrothermal processing of hydroxides of tin and antimony at a temperature of 170C for 48 hours

3. The method according to claim 2, characterized in that the hydroxides of tin and antimony is obtained by dissolution of metallic Sn and Sb in concentrated hydrochloric acid, 18-20 wt.%, with the addition of 3-5 wt.% concentrated HNO3obtained solution is diluted with distilled water 2-3 times and poured the calculated amount of ammonia solution.


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