CN113637943B - Preparation method of photosensitive carbon disulfide sensor - Google Patents

Preparation method of photosensitive carbon disulfide sensor Download PDF

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CN113637943B
CN113637943B CN202110858227.XA CN202110858227A CN113637943B CN 113637943 B CN113637943 B CN 113637943B CN 202110858227 A CN202110858227 A CN 202110858227A CN 113637943 B CN113637943 B CN 113637943B
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silver sulfide
silver
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quartz tube
carbon disulfide
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CN113637943A (en
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董孟孟
蔡庆锋
彭雪
吕燕飞
赵士超
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Hangzhou Dianzi University
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Abstract

The invention discloses a preparation method of a photosensitive carbon disulfide sensor, which comprises the steps of firstly depositing and growing Jin Cha finger electrodes on an alumina ceramic substrate, then coating silver sulfide nano particles on the surfaces of Jin Cha finger electrodes to obtain a silver sulfide detector, arranging the silver sulfide detector in a container, and arranging a blue LED light source in the container. The invention has simple operation, and has very good gas sensitivity to the carbon disulfide through photoexcitation-induced photoelectrochemical reaction.

Description

Preparation method of photosensitive carbon disulfide sensor
Technical Field
The invention belongs to the field of device preparation, and particularly relates to a preparation method of a silver sulfide nanoparticle carbon disulfide sensor.
Background
Silver sulfide materials have a wide range of uses, such as fluorescent materials, gas detection materials. The mechanism is based on that after detected gas molecules are adsorbed on the surface of silver sulfide, electrons on the surface of silver sulfide crystal grains are enriched or exhausted, energy bands on the surface of silver sulfide crystal grains are bent, potential barriers of electron movement are lowered or raised, the resistance of silver sulfide is changed, and detection of the gas molecules is realized. The characteristic of such detectors is that the energy band bending induced barrier is related to the kind and amount of adsorbed gas molecules, and it is difficult to distinguish specific gas kinds for the same type of gas, such as reducing gas.
Disclosure of Invention
The invention provides a preparation method of a photosensitive carbon disulfide sensor aiming at the defects of the prior art.
A preparation method of a photosensitive carbon disulfide sensor comprises the following steps: on an alumina ceramic substrate, a Jin Cha finger electrode is deposited and grown firstly, then silver sulfide nano particles are coated on the surface of the Jin Cha finger electrode, a silver sulfide detector is obtained, the silver sulfide detector is arranged in a container, and a blue LED light source is arranged in the container.
Preferably, the silver sulfide nano-particles are replaced by nano-palladium modified silver sulfide.
Preferably, the preparation method of the silver sulfide nano-particles comprises the following steps:
step (1), depositing a silver film with the thickness of 100-500nm on the surface of a silicon dioxide substrate by a thermal evaporation method;
step (2), putting sulfur powder into a quartz boat, covering a silicon dioxide substrate with silver plated on the surface of the quartz boat, wherein the silver surface is opposite to sulfur; then putting the quartz boat into a quartz tube;
sealing the two ends of the quartz tube in the step (2), and vacuumizing;
step (4), placing the quartz tube in the step (3) into a tubular electric furnace, and heating to 200-300 ℃ at a heating rate of 10-30 ℃/min; the temperature is raised to 200-300 ℃ and then the heat is preserved for 30-120 min;
stopping heating the tubular electric furnace and the quartz tube, starting the tubular electric furnace, rapidly cooling the quartz tube to room temperature in a room temperature environment, and then taking out the substrate to obtain a silver sulfide film on the substrate;
and (6) scraping the silver sulfide film obtained in the step (5) from the growth substrate by a scraper to obtain silver sulfide nano particles.
Preferably, the silver sulfide detector is prepared, and specifically comprises the following steps:
step (1), preparing silver sulfide nano particles with the particle diameter of 10-100nm by a solution method or a chemical gas phase method;
step (2), mixing silver sulfide nano particles with water to form paste, and spin-coating the paste on the surface of an interdigital electrode by a spin-coating method, wherein the substrate of the interdigital electrode is alumina ceramic or a silicon substrate with an oxide layer grown on the surface;
and (3) drying the product obtained in the step (2) in air to remove water, thereby obtaining the silver sulfide detector.
Preferably, the preparation method of the silver sulfide nano-particles comprises the following steps:
step (1), depositing a silver film with the thickness of 100-500nm on the surface of a silicon dioxide substrate by a thermal evaporation method;
step (2), putting sulfur powder into a quartz boat, covering a silicon dioxide substrate with silver plated on the surface of the quartz boat, wherein the silver surface is opposite to sulfur; then putting the quartz boat into a quartz tube;
sealing the two ends of the quartz tube in the step (2), and vacuumizing;
step (4), placing the quartz tube in the step (3) into a tubular electric furnace, and heating to 200-300 ℃ at a heating rate of 10-30 ℃/min; the temperature is raised to 200-300 ℃ and then the heat is preserved for 30-120 min;
stopping heating the tubular electric furnace and the quartz tube, starting the tubular electric furnace, rapidly cooling the quartz tube to room temperature in a room temperature environment, and then taking out the substrate to obtain a silver sulfide film on the substrate;
spraying a palladium chloride hydrochloric acid solution on the surface of the silver sulfide film obtained in the step (5) by a spray method, and forming a palladium chloride liquid film on the surface of the silver sulfide, wherein the palladium chloride hydrochloric acid solution is a mixed solution of a palladium chloride saturated solution and hydrochloric acid;
step (7), putting the product obtained in the step (6) into a quartz tube, introducing argon and hydrogen mixed gas, wherein the volume content of the hydrogen is 5%, and then putting into a tubular electric furnace, and heating to 500-800 ℃ at a heating rate of 10-30 ℃/min; the temperature is raised to 500-800 ℃ and then the heat is preserved for 30-60 min; obtaining nano palladium modified silver sulfide.
Compared with the prior art, the invention has the following effects: the invention has simple operation, and has very good gas sensitivity to the carbon disulfide through photoexcitation-induced photoelectrochemical reaction.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Detailed Description
As shown in fig. 1, the present invention introduces optical excitation by which the potential barrier is altered. The photoelectrochemical gas detector can identify specific gases, such as ethanol, water vapor and carbon disulfide, the property of detection signals of the carbon disulfide is completely different from the property of the specific gases, the resistance of the specific gases is reduced, the resistance of the specific gases is increased, and the identification of the carbon disulfide can be realized.
The nano silver sulfide has large specific surface area, can adsorb a large number of gas molecules, and is beneficial to the detection of low-concentration detected gas. When a small amount of sulfur disulfide gas is contained in the air, silver sulfide preferentially adsorbs the gas to form a compact adsorption layer, gas molecules are in a multi-molecular layer adsorption mode on the surface of the silver sulfide, oxygen in the air can be adsorbed outside the compact layer, and the oxygen adsorption outside the compact layer is mainly due to low carbon disulfide concentration. When the adsorption reaches dynamic balance, the energy level barrier between silver sulfide grains is reduced to a constant value, and the resistance is also reduced to a constant value. When light irradiates on the surface of silver sulfide, the silver sulfide is excited by light to generate photo-generated electron-hole pairs, the chemical reaction of carbon disulfide and oxygen is promoted, the carbon disulfide is reduced along with the reduction of the carbon disulfide of the compact adsorption layer, the potential barrier of the silver sulfide is increased and the resistance is rapidly increased, so that the detection of the carbon disulfide is realized. Unlike carbon disulfide, ethanol and water vapor do not form a tight adsorption layer, and the device does not show the phenomenon after illumination.
Embodiment one:
step (1), depositing a silver film with the thickness of 100nm on the surface of a silicon dioxide substrate by a thermal evaporation method;
step (2), putting sulfur powder into a quartz boat, covering a silicon dioxide substrate with silver plated on the surface of the quartz boat, wherein the silver surface is opposite to sulfur; then putting the quartz boat into a quartz tube;
sealing the two ends of the quartz tube in the step (2), and vacuumizing;
step (4), placing the quartz tube in the step (3) into a tubular electric furnace, and heating to 200 ℃ at a heating rate of 10 ℃/min; keeping the temperature at 200 ℃ for 30min;
stopping heating the tubular electric furnace and the quartz tube, starting the tubular electric furnace, rapidly cooling the quartz tube to room temperature in a room temperature environment, and then taking out the substrate to obtain a silver sulfide film on the substrate;
and (6) scraping the silver sulfide film obtained in the step (5) from the growth substrate by a scraper to obtain silver sulfide nano particles.
Step (7), mixing silver sulfide nano particles with water to form paste, and spin-coating the paste on the surface of an interdigital electrode by a spin-coating method, wherein the substrate of the interdigital electrode is alumina ceramic;
step (8), drying the product of the step (7) in air to remove water to obtain a silver sulfide detector;
and (9) arranging a silver sulfide detector in a glass container, wherein a blue light LED light source is arranged in the glass container.
Embodiment two:
step (1), depositing a silver film with the thickness of 300nm on the surface of a silicon dioxide substrate by a thermal evaporation method;
step (2), putting sulfur powder into a quartz boat, covering a silicon dioxide substrate with silver plated on the surface of the quartz boat, wherein the silver surface is opposite to sulfur; then putting the quartz boat into a quartz tube;
sealing the two ends of the quartz tube in the step (2), and vacuumizing;
step (4), placing the quartz tube in the step (3) into a tubular electric furnace, and heating to 250 ℃ at a heating rate of 15 ℃/min; keeping the temperature at 250 ℃ for 60min;
stopping heating the tubular electric furnace and the quartz tube, starting the tubular electric furnace, rapidly cooling the quartz tube to room temperature in a room temperature environment, and then taking out the substrate to obtain a silver sulfide film on the substrate;
and (6) scraping the silver sulfide film obtained in the step (5) from the growth substrate by a scraper to obtain silver sulfide nano particles.
Step (7), mixing silver sulfide nano particles with water to form paste, and spin-coating the paste on the surface of an interdigital electrode by a spin-coating method, wherein the substrate of the interdigital electrode is alumina ceramic;
step (8), drying the product of the step (7) in air to remove water to obtain a silver sulfide detector;
and (9) arranging a silver sulfide detector in a glass container, wherein a blue light LED light source is arranged in the glass container.
Embodiment III:
step (1), depositing a silver film with the thickness of 500nm on the surface of a silicon dioxide substrate by a thermal evaporation method;
step (2), putting sulfur powder into a quartz boat, covering a silicon dioxide substrate with silver plated on the surface of the quartz boat, wherein the silver surface is opposite to sulfur; then putting the quartz boat into a quartz tube;
sealing the two ends of the quartz tube in the step (2), and vacuumizing;
step (4), placing the quartz tube in the step (3) into a tubular electric furnace, and heating to 300 ℃ at a heating rate of 30 ℃/min; keeping the temperature at 300 ℃ for 120min;
stopping heating the tubular electric furnace and the quartz tube, starting the tubular electric furnace, rapidly cooling the quartz tube to room temperature in a room temperature environment, and then taking out the substrate to obtain a silver sulfide film on the substrate;
and (6) scraping the silver sulfide film obtained in the step (5) from the growth substrate by a scraper to obtain silver sulfide nano particles.
Step (7), mixing silver sulfide nano particles with water to form paste, and spin-coating the paste on the surface of the interdigital electrode by a spin-coating method, wherein the substrate of the interdigital electrode is a silicon substrate with an oxide layer grown on the surface;
step (8), drying the product of the step (7) in air to remove water to obtain a silver sulfide detector;
and (9) arranging a silver sulfide detector in a glass container, wherein a blue light LED light source is arranged in the glass container.
Embodiment four:
step (1), depositing a silver film with the thickness of 100nm on the surface of a silicon dioxide substrate by a thermal evaporation method;
step (2), putting sulfur powder into a quartz boat, covering a silicon dioxide substrate with silver plated on the surface of the quartz boat, wherein the silver surface is opposite to sulfur; then putting the quartz boat into a quartz tube;
sealing the two ends of the quartz tube in the step (2), and vacuumizing;
step (4), placing the quartz tube in the step (3) into a tubular electric furnace, and heating to 300 ℃ at a heating rate of 30 ℃/min; keeping the temperature at 300 ℃ for 120min;
stopping heating the tubular electric furnace and the quartz tube, starting the tubular electric furnace, rapidly cooling the quartz tube to room temperature in a room temperature environment, and then taking out the substrate to obtain a silver sulfide film on the substrate;
spraying a palladium chloride hydrochloric acid solution on the surface of the silver sulfide film obtained in the step (5) by a spray method, and forming a palladium chloride liquid film on the surface of the silver sulfide, wherein the palladium chloride hydrochloric acid solution is a mixed solution of a palladium chloride saturated solution and hydrochloric acid;
step (7), putting the product obtained in the step (6) into a quartz tube, introducing argon and hydrogen mixed gas, wherein the volume content of the hydrogen is 5%, and then putting into a tubular electric furnace, and heating to 800 ℃ at a heating rate of 30 ℃/min; keeping the temperature at 800 ℃ for 60min; obtaining nano palladium modified silver sulfide.
Step (8), mixing nano palladium modified silver sulfide particles with water to form paste, and spin-coating the paste on the surface of an interdigital electrode by a spin-coating method, wherein the substrate of the interdigital electrode is alumina ceramic;
step (9), drying the product obtained in the step (8) in air to remove water to obtain a silver sulfide detector;
and (10) arranging a silver sulfide detector in a glass container, wherein a blue LED light source is arranged in the glass container.
Fifth embodiment:
step (1), depositing a silver film with the thickness of 100nm on the surface of a silicon dioxide substrate by a thermal evaporation method;
step (2), putting sulfur powder into a quartz boat, covering a silicon dioxide substrate with silver plated on the surface of the quartz boat, wherein the silver surface is opposite to sulfur; then putting the quartz boat into a quartz tube;
sealing the two ends of the quartz tube in the step (2), and vacuumizing;
step (4), placing the quartz tube in the step (3) into a tubular electric furnace, and heating to 200 ℃ at a heating rate of 10 ℃/min; keeping the temperature at 200 ℃ for 30min;
stopping heating the tubular electric furnace and the quartz tube, starting the tubular electric furnace, rapidly cooling the quartz tube to room temperature in a room temperature environment, and then taking out the substrate to obtain a silver sulfide film on the substrate;
spraying a palladium chloride hydrochloric acid solution on the surface of the silver sulfide film obtained in the step (5) by a spray method, and forming a palladium chloride liquid film on the surface of the silver sulfide, wherein the palladium chloride hydrochloric acid solution is a mixed solution of a palladium chloride saturated solution and hydrochloric acid;
step (7), putting the product obtained in the step (6) into a quartz tube, introducing argon and hydrogen mixed gas, wherein the volume content of the hydrogen is 5%, and then putting into a tubular electric furnace, and heating to 500 ℃ at a heating rate of 10 ℃/min; keeping the temperature at 500 ℃ for 30min; obtaining nano palladium modified silver sulfide.
Step (8), mixing nano palladium modified silver sulfide particles with water to form paste, and spin-coating the paste on the surface of an interdigital electrode by a spin-coating method, wherein the substrate of the interdigital electrode is alumina ceramic;
step (9), drying the product obtained in the step (8) in air to remove water to obtain a silver sulfide detector;
and (10) arranging a silver sulfide detector in a glass container, wherein a blue LED light source is arranged in the glass container.
Example six:
step (1), depositing a silver film with the thickness of 250nm on the surface of a silicon dioxide substrate by a thermal evaporation method;
step (2), putting sulfur powder into a quartz boat, covering a silicon dioxide substrate with silver plated on the surface of the quartz boat, wherein the silver surface is opposite to sulfur; then putting the quartz boat into a quartz tube;
sealing the two ends of the quartz tube in the step (2), and vacuumizing;
step (4), placing the quartz tube in the step (3) into a tubular electric furnace, and heating to 250 ℃ at a heating rate of 15 ℃/min; keeping the temperature at 250 ℃ for 70min;
stopping heating the tubular electric furnace and the quartz tube, starting the tubular electric furnace, rapidly cooling the quartz tube to room temperature in a room temperature environment, and then taking out the substrate to obtain a silver sulfide film on the substrate;
spraying a palladium chloride hydrochloric acid solution on the surface of the silver sulfide film obtained in the step (5) by a spray method, and forming a palladium chloride liquid film on the surface of the silver sulfide, wherein the palladium chloride hydrochloric acid solution is a mixed solution of a palladium chloride saturated solution and hydrochloric acid;
placing the product obtained in the step (7) into a quartz tube, introducing argon and hydrogen mixed gas, wherein the volume content of the hydrogen is 5%, and then placing into a tubular electric furnace, and heating to 700 ℃ at a heating rate of 17 ℃/min; keeping the temperature after the temperature is raised to 700 ℃, wherein the heat preservation time is 40min; obtaining nano palladium modified silver sulfide.
Step (8), mixing nano palladium modified silver sulfide particles with water to form paste, and spin-coating the paste on the surface of an interdigital electrode by a spin-coating method, wherein the substrate of the interdigital electrode is a silicon substrate with an oxide layer grown on the surface;
step (9), drying the product obtained in the step (8) in air to remove water to obtain a silver sulfide detector;
and (10) arranging a silver sulfide detector in a glass container, wherein a blue LED light source is arranged in the glass container.

Claims (5)

1. The application method of the gas-sensitive carbon disulfide sensor is characterized by comprising the following steps of: the sensor is obtained by depositing and growing Jin Cha finger electrodes on an alumina ceramic substrate, and then coating silver sulfide nano particles on the surfaces of Jin Cha finger electrodes;
the use method of the sensor is that the sensor is arranged in a container with a blue light LED light source, when a small amount of disulfide gas is contained in the air, silver sulfide adsorbs the gas to form a compact adsorption layer, gas molecules are in a multi-molecular layer adsorption mode on the surface of the silver sulfide, oxygen in the air can be adsorbed outside the compact layer, and the oxygen adsorption outside the compact layer is mainly due to low carbon disulfide concentration; when the adsorption reaches dynamic balance, the energy level potential barrier between silver sulfide grains is reduced to a constant value, and the resistance is also reduced to a constant value; when light irradiates the surface of silver sulfide, the silver sulfide is excited by light to generate photo-generated electron-hole pairs, the chemical reaction of carbon disulfide and oxygen is promoted, the carbon disulfide is reduced along with the reduction of the carbon disulfide of the compact adsorption layer, the adsorption of oxygen outside the compact layer is carried out, the potential barrier of the silver sulfide is increased, the resistance is increased sharply, and the detection of the carbon disulfide is realized.
2. The method of using a gas-sensitive carbon disulfide sensor of claim 1, wherein: the silver sulfide nano particles are replaced by nano palladium modified silver sulfide.
3. The method of using a gas-sensitive carbon disulfide sensor of claim 1, wherein: the preparation method of the silver sulfide nano-particles comprises the following steps:
step (1), depositing a silver film with the thickness of 100-500nm on the surface of a silicon dioxide substrate by a thermal evaporation method;
step (2), putting sulfur powder into a quartz boat, covering a silicon dioxide substrate with silver plated on the surface of the quartz boat, wherein the silver surface is opposite to sulfur; then putting the quartz boat into a quartz tube;
sealing the two ends of the quartz tube in the step (2), and vacuumizing;
step (4), placing the quartz tube in the step (3) into a tubular electric furnace, and heating to 200-300 ℃ at a heating rate of 10-30 ℃/min; the temperature is raised to 200-300 ℃ and then the heat is preserved for 30-120 min;
stopping heating the tubular electric furnace and the quartz tube, starting the tubular electric furnace, rapidly cooling the quartz tube to room temperature in a room temperature environment, and then taking out the substrate to obtain a silver sulfide film on the substrate;
and (6) scraping the silver sulfide film obtained in the step (5) from the growth substrate by a scraper to obtain silver sulfide nano particles.
4. The method of using a gas-sensitive carbon disulfide sensor of claim 1, wherein: the preparation method of the silver sulfide detector specifically comprises the following steps:
step (1), preparing silver sulfide nano particles with the particle diameter of 10-100nm by a solution method or a chemical vapor phase method;
step (2), mixing silver sulfide nano particles with water to form paste, and spin-coating the paste on the surface of an interdigital electrode by a spin-coating method, wherein the substrate of the interdigital electrode is alumina ceramic or a silicon substrate with an oxide layer grown on the surface;
and (3) drying the product obtained in the step (2) in air to remove water, thereby obtaining the silver sulfide detector.
5. The method of using a gas-sensitive carbon disulfide sensor according to claim 2, wherein: the preparation method of the silver sulfide nano-particles comprises the following steps:
step (1), depositing a silver film with the thickness of 100-500nm on the surface of a silicon dioxide substrate by a thermal evaporation method;
step (2), putting sulfur powder into a quartz boat, covering a silicon dioxide substrate with silver plated on the surface of the quartz boat, wherein the silver surface is opposite to sulfur; then putting the quartz boat into a quartz tube;
sealing the two ends of the quartz tube in the step (2), and vacuumizing;
step (4), placing the quartz tube in the step (3) into a tubular electric furnace, and heating to 200-300 ℃ at a heating rate of 10-30 ℃/min; the temperature is raised to 200-300 ℃ and then the heat is preserved for 30-120 min;
stopping heating the tubular electric furnace and the quartz tube, starting the tubular electric furnace, rapidly cooling the quartz tube to room temperature in a room temperature environment, and then taking out the substrate to obtain a silver sulfide film on the substrate;
spraying a palladium chloride hydrochloric acid solution on the surface of the silver sulfide film obtained in the step (5) by a spray method, and forming a palladium chloride liquid film on the surface of the silver sulfide, wherein the palladium chloride hydrochloric acid solution is a mixed solution of a palladium chloride saturated solution and hydrochloric acid;
step (7), putting the product obtained in the step (6) into a quartz tube, introducing argon and hydrogen mixed gas, wherein the volume content of the hydrogen is 5%, and then putting into a tubular electric furnace, and heating to 500-800 ℃ at a heating rate of 10-30 ℃/min; the temperature is raised to 500-800 ℃ and then the heat is preserved for 30-60 min; obtaining nano palladium modified silver sulfide.
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CN107478698A (en) * 2017-08-03 2017-12-15 山东理工大学 A kind of preparation method and application of in-situ preparation silver sulfide competitive type aflatoxin optical electro-chemistry sensor
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US10725055B1 (en) * 2016-04-15 2020-07-28 University Of Oregon Compounds for carbonyl sulfide/carbon disulfide/hydrogen sulfide release and methods of making and using the same
CN107478698A (en) * 2017-08-03 2017-12-15 山东理工大学 A kind of preparation method and application of in-situ preparation silver sulfide competitive type aflatoxin optical electro-chemistry sensor
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