Manufacturing method of gas sensor material for detection of carbon monoxide co without heating

FIELD: measurement equipment.

SUBSTANCE: scope of application: for carbon monoxide detection in air. Invention consists in the following: manufacturing method includes obtaining nanocrystalline wide gap semiconducting oxides MeO (SnO2, ZnO, In2O3), obtaining sols of quantum dots of narrow gap semiconductors CdX (X=Se, Te, S) and oxides impregnation with sols of quantum dots followed by drying for formation of heterocontacts MO/CdX.

EFFECT: providing possibility of decrease of semiconductive sensor materials temperature to the room temperature upon detection of carbon monoxide in air and providing high sensitivity and low energy consumption of sensor.

2 cl

 

The technical field to which the invention relates

The invention relates to gas sensors, and specifically to devices, the detecting carbon monoxide (carbon monoxide) in the air. Carbon monoxide CO gas is colorless and odorless, is one of the most toxic air pollutants. The danger of carbon monoxide caused by its ability to chemically communicate with the hemoglobin of the blood is stronger than oxygen, thus blocked the process of oxygen transport and cellular respiration. At concentrations of 0.1% carbon monoxide completely paralyzes the breathing of humans and cause death. Maximum permissible concentration (MPC) of carbon monoxide in the air of working zone is 20 mg/m3(17 ppm). The main sources of carbon monoxide are the processes of incomplete combustion, marked by numerous accidents with fatalities due to carbon monoxide poisoning in the tunnels because of the exhaust of cars and fires. Continuous monitoring of the concentration of carbon monoxide in the air is needed in the outer atmosphere and in space. Increased concentration of carbon monoxide may indicate the occurrence of fire and incomplete combustion of diesel fuel or gas for power generation and industrial installations, boilers of small capacity and in automotive engines internal�th combustion. The high concentration of CO in the air can also be caused by cigarette Smoking, which is especially dangerous in places of a mass congestion of people and transport.

The level of technology

For the detection of toxic gases in the air at the level of the MPC is widely used semiconductor resistive type sensors. 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 as a result of chemical reactions on the surface, for example of the interaction of carbon monoxide with hammarbyhamnen oxygen at a temperature of 250-400°C. the Sensors based on SnO2and ZnO are characterized by high sensitivity, good responsiveness, and a number of other advantages. The design of the sensor includes a sensitive semiconductor layer on a dielectric substrate, a built-in Pt heater deposited as a thin film on the opposite side of the dielectric substrate and the electrical contacts for measuring the conductivity of the sensitive layer and the heater power. The heat sensitive layer is necessary for the activation of chemical reactions on the surface, increasing the conductivity chuvstvitelno� layer and desorption of the reaction products. The need for heat sensitive layer substantially complicates the design of the sensor increases its cost and power consumption. The high temperature of the sensitive layer in the process of detecting carbon monoxide is an additional source of danger, which significantly limits their range of applications, eliminating the use of semiconductor sensors in fire detectors and alarm systems in transport.

For the purpose of lowering the operating temperature of the sensor used catalysts based on platinum group metals (Pd, Pt), which is in the form of clusters is applied to the surface of the sensitive layer. Lower operating temperatures is due to the spill-over effect of the gas molecules and reduce the activation energy of the reaction with hammarbyhamnen oxygen on the catalytic clusters (Gas Sensor Based on Semiconductor Metal Oxides, in Metal Oxides. Chemistry and Applications, Ed. J. L. G. Fierro, Taylor&Francis, 2006, p.683) In some cases it is possible to lower the operating temperature of the sensor to 150°C, however, to completely get rid of the heater upon detection of carbon monoxide fails.

Description analogs

Known sensor device (Publication WO 2006088477 A2 2006) in which to activate the processes of interaction of semiconductor gas instead of heating used source of narrow-band light radiation. It is assumed that in �the parameters by the nature of the gas under various necessary light energy to excite the complex of gas molecules with the surface of the semiconductor. At a certain energy, selective for a pair of semiconductor - analyzed gas, the activation reaction on the surface and the change of the electrical resistance of the sensitive layer is proportional to the concentration of gas in air. A significant disadvantage of the device is its high cost and large size due to the necessity of using narrow-band light sources in the infrared range (lasers) for the excitation of molecular complexes on the surface of the semiconductor.

The closest in technical essence and the achieved effect is the way of the sensor material (Publication WO 2009037289 2009 A1) for detecting the carbon monoxide wereda and vapors of volatile organic compounds in the air without heating, in which to activate the processes of interaction of a sensitive layer with gases, a source of ultraviolet radiation (UV). The sensor in this case includes a layer of nanocrystalline zinc oxide with a grain size of 50-100 nm, deposited on an insulating substrate with the measuring electrodes and a built-in UV light-emitting diode with a wavelength of 360-400 nm. The specified device provides sensitivity to the PPT range of concentrations of carbon monoxide and other organic molecules in the air at room temperature (25°C). Ultraviolet and�radiation causes excitation of electronic levels of zinc oxide, that reduces the electrical resistance of zinc oxide and activation reactions on the surface. The disadvantages of the proposed device are significant the return of electrical properties of zinc oxide in the initial state, usually 10-30 minutes. In addition, the UV radiation may be an additional source of danger when using a sensor in a flammable atmosphere.

Disclosure of invention

The technical result of the present invention is to decrease the operating temperature of the semiconductor sensor materials to room upon detection of carbon monoxide in the air while providing high sensitivity and low power consumption of the sensor.

The implementation of the invention

The task was solved by the present invention. A method of manufacturing a material gas sensor for detection of carbon monoxide in the air WITH no heat, including the production of nanocrystalline wide band gap semiconductor oxides MeO (SnO2, ZnO, In2O3), obtaining a colloidal solution of quantum dots narrow-gap semiconductors CdX (X=Se, Te, S) and impregnated with oxides of the colloidal solution of quantum dots, followed by drying prior to formation of heterocontacts MeO/CdX. In a preferred embodiment, the resulting material is applied on an insulating substrate of polycrystalline oxide� aluminum with a platinum measuring electrode and a built-in light-emitting diode with a wavelength in the range 455-532 nm.

A method of manufacturing a material gas sensor for detection of carbon monoxide is carried out without heating according to the invention by obtaining nanocrystalline ceramics wide band gap semiconductor oxides SnO2, ZnO, In2O3. The resulting material is applied on an insulating substrate made of polycrystalline alumina with the measuring electrodes in the form of a paste with a binder, which is used as a solution of a-terpineol in alcohol, and then produce heating of the paste at a temperature of 450°C-500°C for 6 hours to remove the binder. Sensitization sensitive layer is impregnated oxide Sol and colloidal quantum dots narrow-gap semiconductors CdSe, CdS, CdTe, followed by drying at a temperature of 50°C until the formation of heterocontact quantum dots with a wide band gap matrix.

In a preferred embodiment, the nanocrystalline oxides SnO2, In2O3or ZnO obtained by Sol-gel from aqueous solutions of the corresponding chlorides, nitrates or acetates using as gidrolizuemye agent ammonia solution at pH 7-8. Sols quantum dots obtained by colloidal synthesis using trioctylphosphine (source of selenium) and cadmium oleate (source of cadmium in the environment nonpolar high�okipage organic solvent using as the stabilizer of oleic acid. Impregnation of nanocrystalline oxides by Sol quantum dots was carried out for 60 minutes to achieve a concentration of quantum dots in the oxide matrix is not less than 1 mass%.

It is possible to increase the concentration of quantum dots in oxide matrix using mercaptopropionic acid as a linker for immobilization of quantum dots on the surface of oxide nanocrystals. To this end nanocrystalline oxide matrix was treated with a solution of mercaptopropionic acid in ethanol for 60 minutes at room temperature. After that, the oxide matrix impregnated with the Sol narrow-gap quantum dots of cadmium chalcogenides. It is possible to increase the concentration of quantum dots in oxide matrix to 2.2 wt.%.

As a result of synthesis get sensitized materials consisting of a matrix of semiconductor oxide crystallite size of 3-15 nm to immobilized on the surface of narrow-gap quantum dots of cadmium chalcogenides. The content of the quantum dots in oxide matrix is 1-2 wt.%.

Depending on the composition can be obtained in different sensitized materials: SnO2/CdSe, SnO2/CdTe, SnO2/CdS, ZnO/CdSe, ZnO/CdTe, ZnO/CdS, In2O3/CdSe, In2O3/CdTe, In2O3/CdS.

Obtained in this way sensitized mother�crystals have advantages in creating gas sensors. The introduction of narrow-gap nanocrystals (quantum dots (CdTe, CdSe, CdS) in wide band gap matrix (ZnO SnO2, In2O3) increases the photosensitivity of the material in the visible spectrum, this increases the coefficient of light extinction and increases the efficiency of charge separation in the material. The ability to control the spectral sensitivity of materials by changing the size of quantum dots allows you to control chemical processes on the surface of materials, which is especially important for increasing the selectivity of chemical sensors. Electronic structure of semiconductor heterojunction in this case leads to the fact that the electron and the hole is energetically favorable in different parts of the structure. Varying the sizes of the nanoparticles to control the processes of charge separation and to control not only the spectral position of the optical transition, but also the time of recombination and the extinction coefficients of the. The excitation source can be used built-in light emitting diode with a power of 10 mW.

When exposed on the sensitized material light in the visible spectrum the excitation of electronic levels in narrow-gap quantum dots, which leads to the formation of electron - hole pairs (excitons), the separation of carriers and electron transfer� in the conduction band of the wide-gap oxide, this decreases the conductivity of the material. In the presence of trace concentrations of carbon monoxide in the air, exposure to light leads to the activation of chemical reactions of carbon monoxide with hammarbyhamnen oxygen on the surface of the material at room temperature. The result of these reactions is an additional reduction of the resistance of a material is proportional to the concentration of carbon monoxide, which is measured to determine the sensor signal. In air in the absence of carbon monoxide electrical properties of sensitized materials are returned to the initial state. Repeated Cycling of atmospheric composition: clean air/20 ppm WITH evidence of complete reversibility of the effect of the change in the electrical resistance.

The sensory materials used for the manufacture and testing of gas sensors, materials were applied to microelectronic chip that includes as major elements of the insulating substrate of polycrystalline Al2O3with a platinum measuring electrode and a built-in light emitting diode with a wavelength of 532 nm. The sensitive layer of sensitized materials applied between the measuring electrodes. Sensory properties were determined by measuring the resistance CHUV�twitterlogo layer under exposure to light with a duration of the light pulse 30 sec.

The sensor signal was calculated as the ratio of the conductivity sensor in terms of exposure to light at room temperature in the presence of the carbon monoxide in the air to the conductivity sensor on the air. It is established that proposed by the present invention, the materials exhibit high sensitivity to airborne levels of carbon monoxide at the level of maximum permissible concentrations of the working area.

The invention is illustrated by the following examples:

Example 1. Detection WITH sensitized material SnO2/CdSe at room temperature under conditions of irradiation light emitting diode with a wavelength of 532 nm. For sensitization used CdSe quantum dots having a maximum absorption near 532 nm.

The sensors on the basis of sensitized materials SnO2/CdSe connected to the device for simultaneous measurement of electrical conductivity of 4 sensors were placed in the cell in which you passed the clean air and then a gas mixture containing 20 ppm CO in air. Since carbon monoxide is the gas-reducing agent, in the presence WITH the electrical conductivity of the sensitive layer of n-type conductivity increased, and in an atmosphere of clean air decreased. Detection was performed WITH without heating at room temperature when exposed to light built-in light emitting diode with a wavelength of 532 n�. Investigation of sensory properties were carried out under cyclic change of the air flow and the flow of the gas mixture containing CO. The total gas flow over the sensor remained constant and was 100 ml/min.

Installed:

- as a result of exposure to light in an atmosphere of clean air conductivity sensor, consisting of SnO2without applying a photosensitizer, rose 12 times; conductivity sensor, quantum dots sensitized, increased 10 times.

- as a result of exposure to light in the presence of 20 ppm CO in air conductivity sensor without applying the photosensitizer rose 12 times; conductivity sensor, quantum dots sensitized, increased by 53 times.

Example 2. Detection WITH sensitized material ZnO/CdS at room temperature under conditions of irradiation light emitting diode with a wavelength of 455 nm. For sensitization used CdS quantum dots having a maximum absorption near 470 nm.

Sensors based on nanocrystalline photosensibilisation ZnO was placed in a cell for simultaneous measurement of electrical conductivity of 4 sensors. Through the cell passed the clean air containing CO at a concentration of 240 ppm; total gas flow over the sensor was constant and was 100 ml/min., the Sensors are alternately exposed CBE�and, this was fixed tenovuo conductivity sensor and the conductivity increases under the action of laser radiation.

The experiment is installed:

- as a result of exposure to light in an atmosphere of clean air conductivity sensor, consisting of ZnO without applying a photosensitizer, increased 15-fold; a conductivity sensor, quantum dots sensitized increased 18-fold.

- as a result of exposure to light in air containing 240 ppm CO, conductivity sensor without applying a photosensitizer, has increased 20 times, conductivity sensor, quantum dots sensitized, increased by 177 times.

1. A method of manufacturing a material gas sensor for detection of carbon monoxide in the air WITH no heat, including the production of nanocrystalline wide band gap semiconductor oxides MeO (SnO2, ZnO, In2O3), obtaining a colloidal solution of quantum dots narrow-gap semiconductors CdX (X=Se, Te, S) and impregnated with oxides of the colloidal solution of quantum dots, followed by drying prior to formation of heterocontacts MeO/CdX.

2. A method according to claim 1, characterized in that the material is additionally applied to an insulating substrate made of polycrystalline alumina with a platinum measuring electrode and a built-in light emitting diode with a length �any in the range 455-532 nm.



 

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