CN113249685A - Preparation method of silver sulfide film gas sensor - Google Patents

Preparation method of silver sulfide film gas sensor Download PDF

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Publication number
CN113249685A
CN113249685A CN202110381490.4A CN202110381490A CN113249685A CN 113249685 A CN113249685 A CN 113249685A CN 202110381490 A CN202110381490 A CN 202110381490A CN 113249685 A CN113249685 A CN 113249685A
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silver sulfide
silver
quartz tube
temperature
putting
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董孟孟
吕燕飞
赵士超
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Hangzhou Dianzi University
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/04—Coating on selected surface areas, e.g. using masks
    • C23C14/042—Coating on selected surface areas, e.g. using masks using masks
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5846—Reactive treatment
    • C23C14/5866—Treatment with sulfur, selenium or tellurium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C23C18/42—Coating with noble metals
    • C23C18/44—Coating with noble metals using reducing agents
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means

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Abstract

The invention discloses a preparation method of a silver sulfide film gas-sensitive sensor, which comprises the steps of firstly depositing and growing a silver film on a silicon dioxide substrate, then carrying out gas-phase vulcanization to generate a silver sulfide film, then growing palladium nano particles on the surface of the silver sulfide, and then carrying out vacuum coating and evaporation plating on a platinum interdigital electrode to obtain the palladium-modified silver sulfide gas-sensitive sensor. The palladium modified silver sulfide is used as a gas sensitive layer, and has better gas sensitivity to sulfur-containing gas.

Description

Preparation method of silver sulfide film gas sensor
Technical Field
The invention belongs to the field of device preparation, and particularly relates to a preparation method of a palladium modified silver sulfide film gas sensor.
Background
The silver sulfide is a semiconductor material, has good fluorescence performance and photoelectric performance, and can be used in the fields of fluorescence imaging and near infrared photoelectric detection. In addition, silver sulfide also shows good gas-sensitive performance, can be used in the field of gas sensors, and compared with oxide gas sensors, silver sulfide gas sensors are less researched. Silver sulfide has good selectivity to sulfur-containing gas, and the gas-sensitive performance is improved after noble metal modification.
Disclosure of Invention
According to the invention, a silver film is firstly deposited and grown on a silicon dioxide substrate, then a silver sulfide film is generated through gas phase vulcanization, palladium nano particles are grown on the surface of the silver sulfide, and then a platinum interdigital electrode is evaporated through vacuum coating to obtain the palladium modified silver sulfide gas sensor.
The invention relates to a preparation method of a silver sulfide film gas sensor, which comprises the following specific steps:
depositing a silver film with the thickness of 100-;
and (2) putting the sulfur powder into a quartz boat, covering the surface of the quartz boat with a silicon dioxide substrate with silver plated on the surface, wherein the silver surface is opposite to the sulfur. Then putting the quartz boat into a quartz tube;
sealing two ends of the quartz tube obtained in the step (2), and vacuumizing;
step (4), putting the quartz tube obtained in the step (3) into a tube-type electric furnace, heating to 200-300 ℃, wherein the heating rate is 10-30 ℃/min; keeping the temperature after the temperature is increased to 200-300 ℃, wherein the heat preservation time is 30-120 min;
and (5) 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, taking out the substrate, and obtaining the silver sulfide film on the substrate.
Spraying a hydrochloric acid solution of palladium chloride on the surface of the silver sulfide film obtained in the step (5) by a spraying method to form a liquid film of the palladium chloride on the surface of the silver sulfide, wherein the hydrochloric acid solution of the palladium chloride is a mixed solution of a saturated solution of the palladium chloride and hydrochloric acid;
putting the product obtained in the step (6) into a quartz tube, introducing mixed gas of argon and hydrogen, wherein the volume content of hydrogen is 5%, then putting the quartz tube into a tubular electric furnace, heating to 500-800 ℃, and heating at a rate of 10-30 ℃/min; after the temperature is increased to 500-800 ℃, the temperature is preserved for 30-60 min; obtaining the nano palladium modified silver sulfide.
Step (8), evaporating a platinum interdigital electrode on the surface of the product palladium modified silver sulfide obtained in the step (7) through a template; and finishing the preparation of the device.
Preferably, the temperature for heat preservation in the step (3) is 260-270 ℃.
Preferably, the temperature rise rate in the step (3) is 15-20 ℃/min.
Preferably, the temperature for heat preservation in the step (7) is 600-720 ℃.
Preferably, the temperature rise rate in the step (7) is 15 to 20 ℃/min.
Compared with the prior art, the invention has the following effects: the palladium modified silver sulfide is used as a gas sensitive layer, and has better gas sensitivity to sulfur-containing gas.
Detailed Description
The first embodiment is as follows:
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 the surface of the quartz boat with a silicon dioxide substrate with silver plated on the surface, wherein the silver surface is opposite to sulfur; then putting the quartz boat into a quartz tube;
sealing two ends of the quartz tube obtained in the step (2), and vacuumizing;
step (4), putting the quartz tube in the step (3) into a tube-type electric furnace, heating to 200 ℃, wherein the heating rate is 10 ℃/min; keeping the temperature for 30min after the temperature is raised to 200 ℃;
and (5) 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, taking out the substrate, and obtaining the silver sulfide film on the substrate.
Spraying a hydrochloric acid solution of palladium chloride on the surface of the silver sulfide film obtained in the step (5) by a spraying method to form a liquid film of the palladium chloride on the surface of the silver sulfide, wherein the hydrochloric acid solution of the palladium chloride is a mixed solution of a saturated solution of the palladium chloride and 0.5mol/L hydrochloric acid, and the volume ratio of the hydrochloric acid solution of the palladium chloride to the hydrochloric acid solution of the palladium chloride is 10: 1;
putting the product obtained in the step (6) into a quartz tube, introducing mixed gas of argon and hydrogen, wherein the volume content of hydrogen is 5%, then putting the quartz tube into a tubular electric furnace, heating to 500 ℃, and heating at a rate of 10 ℃/min; keeping the temperature for 30min after the temperature is raised to 500 ℃; obtaining the nano palladium modified silver sulfide.
Step (8), evaporating a platinum interdigital electrode on the surface of the product palladium modified silver sulfide obtained in the step (7) through a template; and obtaining the silver sulfide film gas sensor.
Example two:
depositing a silver film with the thickness of 300nm on the surface of a silicon dioxide substrate by a thermal evaporation method;
and (2) putting the sulfur powder into a quartz boat, covering the surface of the quartz boat with a silicon dioxide substrate with silver plated on the surface, wherein the silver surface is opposite to the sulfur. Then putting the quartz boat into a quartz tube;
sealing two ends of the quartz tube obtained in the step (2), and vacuumizing;
step (4), putting the quartz tube in the step (3) into a tube-type electric furnace, and heating to 260 ℃ at a heating rate of 15 ℃/min; keeping the temperature for 80min after the temperature is increased to 260 ℃;
and (5) 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, taking out the substrate, and obtaining the silver sulfide film on the substrate.
Spraying a hydrochloric acid solution of palladium chloride on the surface of the silver sulfide film obtained in the step (5) by a spraying method to form a liquid film of the palladium chloride on the surface of the silver sulfide, wherein the hydrochloric acid solution of the palladium chloride is a mixed solution of a saturated solution of the palladium chloride and 0.1mol/L hydrochloric acid, and the volume ratio of the hydrochloric acid solution of the palladium chloride to the hydrochloric acid solution of the palladium chloride is 5: 1;
putting the product obtained in the step (6) into a quartz tube, introducing mixed gas of argon and hydrogen, wherein the volume content of hydrogen is 5%, then putting the quartz tube into a tubular electric furnace, heating to 600 ℃, and heating at a rate of 15 ℃/min; keeping the temperature for 40min after the temperature is raised to 600 ℃; obtaining the nano palladium modified silver sulfide.
Step (8), evaporating a platinum interdigital electrode on the surface of the product palladium modified silver sulfide obtained in the step (7) through a template; and obtaining the silver sulfide film gas sensor.
Example three:
depositing a silver film with the thickness of 500nm on the surface of a silicon dioxide substrate by a thermal evaporation method;
and (2) putting the sulfur powder into a quartz boat, covering the surface of the quartz boat with a silicon dioxide substrate with silver plated on the surface, wherein the silver surface is opposite to the sulfur. Then putting the quartz boat into a quartz tube;
sealing two ends of the quartz tube obtained in the step (2), and vacuumizing;
step (4), putting the quartz tube in the step (3) into a tube-type electric furnace, and heating to 300 ℃ at a heating rate of 30 ℃/min; keeping the temperature after the temperature is raised to 300 ℃, wherein the heat preservation time is 120 min;
and (5) 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, taking out the substrate, and obtaining the silver sulfide film on the substrate.
And (6) spraying a hydrochloric acid solution of palladium chloride on the surface of the silver sulfide film obtained in the step (5) by a spraying method to form a liquid film of the palladium chloride on the surface of the silver sulfide, wherein the hydrochloric acid solution of the palladium chloride is a mixed solution of a saturated solution of the palladium chloride and 0.3mol/L hydrochloric acid, and the volume ratio of the hydrochloric acid solution of the palladium chloride to the hydrochloric acid solution of the palladium chloride is 8: 1.
Putting the product obtained in the step (6) into a quartz tube, introducing mixed gas of argon and hydrogen, wherein the volume content of hydrogen is 5%, then putting the quartz tube into a tubular electric furnace, heating to 800 ℃, and heating at the rate of 30 ℃/min; keeping the temperature after the temperature is raised to 800 ℃, wherein the heat preservation time is 60 min; obtaining the nano palladium modified silver sulfide.
Step (8), evaporating a platinum interdigital electrode on the surface of the product palladium modified silver sulfide obtained in the step (7) through a template; and obtaining the silver sulfide film gas sensor.

Claims (5)

1. A preparation method of a silver sulfide film gas sensor is characterized by comprising the following steps:
depositing a silver film with the thickness of 100-;
step (2), putting sulfur powder into a quartz boat, covering the surface of the quartz boat with a silicon dioxide substrate with silver plated on the surface, wherein the silver surface is opposite to sulfur; then putting the quartz boat into a quartz tube;
sealing two ends of the quartz tube obtained in the step (2), and vacuumizing;
step (4), putting the quartz tube obtained in the step (3) into a tube-type electric furnace, heating to 200-300 ℃, wherein the heating rate is 10-30 ℃/min; keeping the temperature after the temperature is increased to 200-300 ℃, wherein the heat preservation time is 30-120 min;
step (5), 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, taking out the substrate, and obtaining a silver sulfide film on the substrate;
spraying a hydrochloric acid solution of palladium chloride on the surface of the silver sulfide film obtained in the step (5) by a spraying method to form a liquid film of the palladium chloride on the surface of the silver sulfide; the hydrochloric acid solution of the palladium chloride is a mixed solution of saturated solution of the palladium chloride and hydrochloric acid;
putting the product obtained in the step (6) into a quartz tube, introducing mixed gas of argon and hydrogen, wherein the volume content of hydrogen is 5%, then putting the quartz tube into a tubular electric furnace, heating to 500-800 ℃, and heating at a rate of 10-30 ℃/min; after the temperature is increased to 500-800 ℃, the temperature is preserved for 30-60 min; obtaining the nano palladium modified silver sulfide.
Step (8), evaporating a platinum interdigital electrode on the surface of the product palladium modified silver sulfide obtained in the step (7) through a template; and finishing the preparation of the device.
2. The method for preparing the silver sulfide thin film gas sensor according to claim 1, wherein the method comprises the following steps: the temperature of the heat preservation in the step (3) is 260-270 ℃.
3. The method for preparing the silver sulfide thin film gas sensor according to claim 1, wherein the method comprises the following steps: the heating rate in the step (3) is 15-20 ℃/min.
4. The method for preparing the silver sulfide thin film gas sensor according to claim 1, wherein the method comprises the following steps: the temperature of the heat preservation in the step (7) is 600-720 ℃.
5. The method for preparing the silver sulfide thin film gas sensor according to claim 1, wherein the method comprises the following steps: the heating rate in the step (7) is 15-20 ℃/min.
CN202110381490.4A 2021-04-09 2021-04-09 Preparation method of silver sulfide film gas sensor Pending CN113249685A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114162849A (en) * 2021-12-08 2022-03-11 杭州电子科技大学 Preparation method of silver sulfide nano material and gas sensitive device
CN118080877A (en) * 2024-04-26 2024-05-28 朗峰新材料启东有限公司 Nanocrystalline particles for sensor and preparation method thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114162849A (en) * 2021-12-08 2022-03-11 杭州电子科技大学 Preparation method of silver sulfide nano material and gas sensitive device
CN114162849B (en) * 2021-12-08 2024-04-12 杭州电子科技大学 Preparation method of silver sulfide nano material and gas-sensitive device
CN118080877A (en) * 2024-04-26 2024-05-28 朗峰新材料启东有限公司 Nanocrystalline particles for sensor and preparation method thereof

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Application publication date: 20210813