Method of producing gas sensor material for selective detection of h2s and derivatives thereof

FIELD: chemistry.

SUBSTANCE: invention comprises producing nano-heterogeneous material based on whisker crystals of n-type oxides SnO2, ZnO, In2O3 and nano-clusters of p-type oxides CuO, NiO, Co3O4 immobilised on the surface of said crystals. The method includes producing whisker crystals from vapour and impregnating the crystals with salt solutions, followed by annealing to form p-n heterocontacts.

EFFECT: high selective sensitivity of the sensor to H2S and derivatives thereof in air.

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The technical field to which the invention relates.

The invention relates to gas sensors, and specifically to devices, the detecting hydrogen sulfide and its derivatives in the air. Hydrogen sulfide (H2S is a product of decomposition of organic and biological substances, is a gas with an unpleasant pungent smell, is one of the most toxic air pollutants with a wide range of toxic effects on humans and animals. On the level of concentration of 170 mg/m3hydrogen sulphide is completely paralyzes the sense of smell of a man from 30 to 50 seconds, at higher concentrations, hydrogen sulfide blocks the lungs and cause death. Maximum permissible concentration (MPC) of hydrogen sulfide in the air of working zone is 10 mg/m3(7.1 ppm).

The level of technology

For detection of toxic gases in the air at the level of the MPC is widely used semiconductor sensors resistive type. The most widespread sensory devices based on thin films of nanocrystalline tin dioxide SnO2and zinc oxide ZnO. The mechanism of action of these devices is based on the change of electrical conductivity of the sensor layer in the course of what is happening on its surface chemical reactions, for example the interaction of hydrogen sulfide with hammarbyhamnen oxygen. Sensoria basis SnO 2and ZnO are characterized by high sensitivity, low cost, good responsiveness and a number of other advantages. At the same time, their typical disadvantages are low selectivity and lack of stability. The main reason for low selectivity is the presence of surface oxides SnO2and ZnO active centers of different nature, which cause the response of sensitive material by various gases in the atmosphere. The low stability of the response of sensors with long-term use caused, first of all, material degradation, the growth of grains of nanocrystalline oxides at the temperature detection. To improve selectivity in sensory devices used modifiers based on platinum group metals, which are in the form of clusters applied to the surface of the grains of a semiconductor oxide. The stability of the sensors can be improved by changing the structure of the sensitive layer with polycrystalline to monocrystalline structure whiskers SnO2or ZnO (I. A. Myasnikov, V. L. Shrew, L. Y. Kupriyanov, S. A. Zavialov. Semiconductor sensors in physico-chemical studies, M.: Nauka, 1991).

Known touch device (U.S. Patent No. 3,901,067, 1975) for indication of hydrogen sulfide, comprising an insulating substrate with the measuring electrodes, rustically layer of polycrystalline tin oxide, doped with aluminium, of a thickness of 4000 Å and the heating element. The specified device provides sensitivity to the concentration of 1 ppm hydrogen sulfide in air at moderate temperatures of the heating element (130°C). The disadvantages of the proposed device is a significant return to its original state, usually a few minutes. To improve the dynamic properties of the sensor increase the operating temperature to 400°C, resulting in non-repeatable measurements and significantly reduces the time the guaranteed operation of the sensor.

Describes a sensor device for indication of hydrogen sulfide on the basis of many individual ZnO whiskers with a diameter of 30 nm, fixed on the substrate and connected two electrical contacts at opposite ends of the nanowires (U.S. Patent No. 8030185, B2, 2011). The method is applied to the threads at the same time many small Islands with a diameter of 10-50 nm of various metals: platinum (Pt), palladium (Pd), Nickel (Ni) and cobalt (Co). The use of solid filiform nanocrystals avoids degradation patterns and significantly increase the value of the specific surface of the sensitive layer. The presence at the same time on the surface of the whiskers islets different nature of catalytic metals significantly increases the sensitivity of the Mat is Rial to toxic gases and allows to detect low total concentration of harmful pollutants in the air. The method relates to gas sensors, which measure the resistance of the array whiskers coated islets of metals in air containing gaseous impurities. The disadvantage of this method is a significant limitation in the selectivity of the sensor, especially when the detection of gaseous reducing agents CO, H2S, NH3. Despite the high sensitivity it is impossible in the signal of a sensor to distinguish the contribution of a particular group of substances, for example, sulfur-containing molecules, which is a serious drawback, especially when monitoring air quality in large cities, in places of a mass congestion of people near chemical plants and refineries oil and gas.

The closest in technical essence and the achieved effect is the way of the sensor material (U.S. Patent No. 20120097917 A1, 2012), in which the active component is set (system) of nanowires of zinc oxide ZnO or tin oxide SnO2coated clusters of noble metals Au, Pt, Pd. Threads vertically fixed on the insulating substrate with contacts. The advantage of the device is its high sensitivity to hydrogen sulfide concentrations at the ppb level and low (room) temperature. The sensitive layer is also characterized by high stability of the structure. Things the public the disadvantage of this device is its low selectivity, the sensor responds to the presence in the air not only H2S, but also other gases-reducing agents CO, NH3N2and gas-oxidizer NO2. To improve the selectivity is proposed to analyze the response time of the sensor simultaneously with the change in conductivity. However, in the case of a mixture of gases to highlight the contribution of a pollutant is not possible.

Disclosure of inventions

The technical effect of the present invention is to improve the selectivity of the semiconductor touch materials for the detection of hydrogen sulfide and its derivatives in the air while providing high sensitivity and stability of the structure of the sensitive layer of the sensor.

The task was solved by the present invention. A method of manufacturing a material gas sensor for the selective detection of H2S and its derivatives is carried out according to the invention receiving whiskers SnO2, ZnO, In2O3the conductivity of n-type, impregnation of these crystals with solutions of salts of Cu, Ni, Co, followed by annealing prior to the formation of oxides CuO, NiO, Co3O4the conductivity of p-type and formation of p-n heterocontacts. The resulting material is preferably applied on the insulating substrate made of polycrystalline alumina with a platinum measuring electrode is but the obverse and a platinum thin film heater on the back side. The resulting material is also preferably applied in paste form with a binder, which is used as a solution of a-terpineol in alcohol, after which produce heating of the paste at a temperature of 450°-500°C for 6 hours to remove the binder.

The implementation of the invention

In a preferred embodiment of the invention whiskers SnO2, In2O3or ZnO is obtained from the vapor on a substrate of polycrystalline Al2O3in a horizontal flow reactor at a temperature of condensation of 950°C To 1030°C in an atmosphere of inert gas with an oxygen content of 0.05-0.1%. Coating the surface of the whiskers clusters of oxides of copper, Nickel and cobalt carried out by impregnation of many whiskers solutions of acetates or nitrates of the metals, followed by drying at a temperature of 100°C and annealing in oxygen atmosphere at a temperature of 250°C for 24 hours. After annealing whiskers is separated mechanically from the substrate.

You can obtain nanowires SnO2, In2OCor ZnO and application of the clusters of oxides of copper, Nickel and cobalt on the surface by chemical vapor deposition from the vapor (CVD) in a vacuum reactor using alcoholate and complex compounds as precursors. As the original substances using the volatile alcoholate and complex compounds, such as di - and Tetra-tert-butylate tin: Sn(OtBu)2and Sn(OtBu)4, acetylacetonates and other Synthesis of nanowires is carried out in high vacuum (10-6mbar). The evaporation temperature of the metal organic precursor is 50-200°C, condensing temperature of 500-800°C.

As a result of synthesis get nanoheterogeneous materials consisting of whiskers semiconductor oxide n-type conductivity with an immobilized on their surface clusters of metal oxide p-type conductivity. The content of oxides of p-type conductivity in nanoheterogeneous materials is 0.6-0.8 mol.%.

Depending on the composition can be obtained by a variety of sensory materials: SnO2/CuO, SnO2/NiO, SnO2/Co3O4, ZnO/Co3O4, ZnO/CuO, ZnO/NiO, In2O3/Co3O4, In2O3/CuO, In2O3/NiO.

Obtained by this method, the materials are characterized by the presence on the surface of filamentous crystal system p-n heterocontacts that form energy barriers for the transport of electrons. The consequence of the formation of p-n junctions is a significant increase in electrical resistance whiskers in an atmosphere of clean air. In the presence of trace concentrations of hydrogen sulfide in the air on the surface of the threads when the temperature is 150-350°C is selective chemical reaction of interaction of clusters of oxides of p-type conductivity of CuO, NiO, Co3O4with hydrogen sulfide, which leads to the formation of well-conducting electric current sulphides of metals. The result of this reaction is the removal of p-n junctions and associated energy barriers for the transport of electrons and as a consequence of the sharp decrease in the resistance of the filaments. On the air in the absence of hydrogen sulfide electrical properties of the whiskers are returned to the initial state in the reverse reaction of interaction of sulfides of metals with oxygen to form oxides CuO, NiO, Co3O4p-type conductivity. Repeated Cycling of the composition of the atmosphere: clean air/10 ppm H2S shows the complete reversibility of the effect of the change in the electrical resistance. It is established that filamentary crystals of n-type conductivity SnO2, ln2O3, ZnO in terms of trace hydrogen sulfide concentration and temperature of 150-350°C do not enter into reaction with the hydrogen sulfide with the formation of sulphides.

Received touch materials used for the manufacture and testing of gas sensors, materials were applied to microelectronic chip, which includes as main elements of the insulating substrate of polycrystalline A12O3with a platinum measuring electrode on the front side and platinum Templin cnym heater on the back side. Sensitive layer on the basis of the whiskers was applied between the measuring electrodes. Sensory properties were determined by measuring the resistance of the sensitive layer, depending on the concentrations of hydrogen sulfide.

The sensor signal was calculated as the ratio of the conductivity sensor in the presence of hydrogen sulfide in the air to the conductivity sensor on the air. It is found that the present invention materials exhibit high sensitivity to the content in the air of hydrogen sulfide and its derivatives at the level of maximum permissible concentration of the working area.

Example 1. Detection of H2S filamentary crystals SnO2and nanoheterogeneous materials SnO2/CuO, SnO2/NiO, SnO2/Co3O4

Sensor array-based whiskers SnO2and nanoheterogeneous materials SnO2/CuO, SnO2/NiO, SnO2/Co3O4connected to the device for simultaneous measurement of electrical conductivity of 4 sensors were placed in the cell in which let in fresh air and gas mixture containing 2 ppm H2's in the air. As H2's gas-reducing agent, in the presence of hydrogen sulfide, the conductivity of the sensitive layer of n-type conductivity increased, and in the atmosphere of the clean air decreased. Detection of H2's conducted is at a temperature of 300°C. The study of sensory properties were conducted under cyclic change of the air flow and the flow of the gas mixture containing H2S. the Total gas flow over the sensor remained constant at 100 ml/min

The experiment established that the touch signal, calculated as described above 2 ppm H2S when applied to the surface of the n threads-SnO2clusters R-CuO increases in 21 times, when applying cluster p-NiO - 13 times and during application clusters R-Co3O4- 28 times.

Example 2. Detection of gases reductants CO and NH3and gas oxidizer NO2filamentary crystals SnO2and nanoheterogeneous materials SnO2/Co3O4

Sensor array-based whiskers SnO2and nanoheterogeneous materials 8nO2/Co3O4connected to the device for measuring conductivity, was placed in a cell in which consistently missed the fresh air and then a gas mixture containing 21 ppm NH3in the air, 14.1 ppm CO in air or 1.7 ppm NO2in the air. The exposure time of the sensor in the atmosphere of pollutants was 5 minutes in clean air for 15 minutes. Since NH3and WITH gaseous reducing agents, their presence in the air leads to an increased value of the conductivity of the sensitive layer of n-type conductivity compared elektroprovodnostju in clean air, while the presence of gas in the air as oxidant NO2leads to a decrease in the magnitude of the conductivity. Detection was performed at a temperature of 300°C. the Total gas flow over the sensor remained constant at 100 ml/min

The experiment was established, in all cases, when applied to the surface of the n threads-SnO2clusters R-Co3O4the touch signal decreases: in the case of detection FROM 10 times, when the detection of NH31.2 times and the detection of NO280 times.

1. A method of manufacturing a material gas sensor for the selective detection of H2S and its derivatives in the air, including the production of whiskers conductivity n-type on the basis of SnO2, ZnO, In2About3the impregnation of these crystals with solutions of salts of Cu, Ni, Co and subsequent annealing before forming the oxide conductivity of p-type CuO, NiO, Co3About4and the formation of p-n heterocontacts.

2. The method according to p. 1, characterized in that the material is additionally applied on the insulating substrate made of polycrystalline alumina with a platinum measuring electrode on the front side and the platinum thin film heater on the reverse side.

3. The method according to p. 1, characterized in that the material is applied in paste form with a binder, as the cat is, which requires a solution of a-terpineol in alcohol, then produce heating the paste at a temperature of 450°C for 6 hours to remove the binder.



 

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