AU2021101870A4 - A facile method to prepare gas sensing materials based on graphene-ZrO2 composites - Google Patents
A facile method to prepare gas sensing materials based on graphene-ZrO2 composites Download PDFInfo
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- 238000000034 method Methods 0.000 title abstract description 13
- 239000011540 sensing material Substances 0.000 title description 7
- 239000007789 gas Substances 0.000 abstract description 57
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract description 47
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 46
- 238000006243 chemical reaction Methods 0.000 abstract description 32
- 229910021389 graphene Inorganic materials 0.000 abstract description 27
- 239000002245 particle Substances 0.000 abstract description 14
- 229910052799 carbon Inorganic materials 0.000 abstract description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 10
- 239000001257 hydrogen Substances 0.000 abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 5
- 150000002894 organic compounds Chemical class 0.000 abstract description 4
- 239000004065 semiconductor Substances 0.000 abstract description 4
- 238000004880 explosion Methods 0.000 abstract description 3
- 239000002360 explosive Substances 0.000 abstract description 3
- 231100000572 poisoning Toxicity 0.000 abstract description 3
- 230000000607 poisoning effect Effects 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000005229 chemical vapour deposition Methods 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 description 4
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 230000005476 size effect Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002800 charge carrier Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0211—Compounds of Ti, Zr, Hf
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- 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
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
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Abstract
As a kind of equipment to detect gas composition and concentration, gas-sensitive
semiconductors are widely used in the detection of inflammable, explosive or harmful
gases in factories, workshops and mines, to ensure the safety of life and property by
preventing the disaster of fire, explosion and poisoning. As the core of sensors, gas
sensitive materials determine the performance of sensors. In this patent, we propose a
method to prepare graphene/ZrO2 composites for gas sensing applications. By placing
ZrO2 particles in plasma reaction zone, methane or other organic compounds are
introduced into the reaction system. Under the aid of hydrogen plasma, graphene can
be easily and quickly synthesized on ZrO2 particles. This method can directly prepare
graphene on ZrO2 particles to obtain graphene-coated ZrO2 with a larger specific
surface area and a high surface carrier concentration, which makes it very sensitive to
the surrounding environments. It provides a simple way to realize the preparation of
carbon-coated ZrO2 composites which can be used in gas sensing devices where the
adsorption or release of one gas molecule can be detected.
1
Description
As a kind of equipment to detect gas composition and concentration, gas-sensitive semiconductors are widely used in the detection of inflammable, explosive or harmful gases in factories, workshops and mines, to ensure the safety of life and property by preventing the disaster of fire, explosion and poisoning. As the core of sensors, gas sensitive materials determine the performance of sensors. In this patent, we propose a method to prepare graphene/ZrO2 composites for gas sensing applications. By placing ZrO2 particles in plasma reaction zone, methane or other organic compounds are introduced into the reaction system. Under the aid of hydrogen plasma, graphene can be easily and quickly synthesized on ZrO2 particles. This method can directly prepare graphene on ZrO2 particles to obtain graphene-coated ZrO2 with a larger specific surface area and a high surface carrier concentration, which makes it very sensitive to the surrounding environments. It provides a simple way to realize the preparation of carbon-coated ZrO2 composites which can be used in gas sensing devices where the adsorption or release of one gas molecule can be detected.
1. Background and Purpose
As a device for detecting gas composition and concentration, gas sensors are widely used in the detection of various flammable, explosive or harmful gases in factories, workshops and mines, and the detection of household flammable gas leakage, so as to achieve the protection of fire, explosion and poisoning, to ensure the safety of life and property. As the core of sensors, the gas-sensitive materials determine the detecting performance of sensors. Electrons are exchanged between the gas adsorbed on the semiconductor surface and the semiconductor, which causes the variety of resistivity, surface potential and rectification characteristics.
Graphene has a unique two-dimensional atomic layer structure, high electron mobility and large specific surface area, making it an ideal gas-sensitive material. First of all, graphene has a large theoretical specific surface area (2630M 2 /G). All the atoms of a single-layer graphene sheet can be considered as surface atoms and molecules that can adsorb gases, providing the largest sensing area per unit volume. Secondly, the charge carriers of graphene have a rest mass of zero close to its Dirac point and graphene exhibits a significantly higher carrier mobility at room temperature, making graphene more conductive than silver. At the same time, graphene has inherently low electrical noise. Due to its high-quality crystal lattice and its two-dimensional structure, it can shield more charge fluctuations than one-dimensional counterparts. A tiny variety in the resistance of the graphene sheet caused by the gas adsorption even dropped to the molecular level is detectable. ZrO2 has good permeability to visible light, excellent chemical stability in aqueous solution, and has specific conductivity and reflect infrared radiation characteristics, so it is widely used in lithium batteries, solar cells, liquid crystal displays, optoelectronic devices, transparent conductive Electrodes, infrared detection protection and other fields. Due to the small size effect, quantum size effect, surface effect and macroscopic quantum tunneling effect, ZrO2 nanomaterial has significant advantages at the physical properties of light, heat, electricity, sound, magnetism and other macroscopic properties compared with traditional ZrO2, by using which, the performance of sensor devices can be improved.
In the years since graphene was discovered, people have been constantly thinking of ways to open up its application fields. It is undoubtedly a promising way to combine with other materials. The application of metal oxides for gas sensing is relatively mature, but there are still many problems that have not been resolved, such as selectivity, operating temperature, stability, and working under oxygen-free conditions. To overcome the above problems, in the patent, we propose a microwave plasma chemical vapor deposition (MPCVD) method to synthesize graphene/ ZrO2 composites for gas sensors.
2. Description of the method to prepare gas sensing materials based on graphene/ZrO2 composites
2.1 The procedure of the preparation of gas sensing materials based on graphene/ZrO2composites
Step 1: To place ZrO2 particles with a diameter of 50-100nm into the reaction tube in the Microwave Plasma Chemical Vapor Deposition (MPCVD) device.
Step 2: To control the vacuum chamber at a pressure of 100150mbar.
Step 3: To carry the carbon sources with a flow rate of 10-100sccm by the working gas with a flow rate of 100-200sccm, which is going to be hydrogen, argon or the mixture of both, into the area where the microwave plasma reaction occurs. The carbon sources described are going to be one or several kinds of organic compounds containing carbon atoms of SP 3 or SP 2 such as methane, methanol, ethanol or methyl formate.
Step 4: To turn on the power supply of the MPCVD device and start the reaction to deposit graphene on ZrO2 particles with a growth time of 5-60 minutes.
Step 5: After the reaction, the graphene/ZrO2 composites with a high specific surface area is obtained.
Step 6: To characterize the gas sensing properties of the synthesized graphene/ZrO2 composites.
2.2 The components ofthe Microwave Plasma Chemical Vapor Deposition system for growing gas sensing materials based on graphene/ZrO2composites
A microwave source with a power range of 0.5-kW is used to provide the microwave plasma. A reaction tube with a diameter of 2050mm are arranged inside the microwave source as reaction and protective chamber. A gas inlet pipe and a gas outlet pipe are connected with each end of the reaction tube for the inlet and outlet of gas respectively. A vacuum pump is employed to pump out the gas inside the reaction tube. A barometer is connected to the gas inlet pipe to monitor the pressure inside the tube. Two valves (valve I and valve II, see Fig. 1) are connected to the gas inlet pipe and gas outlet pipe to control the gas in/out or not respectively.
2.3 The procedure of the control of two valves
Step 1: To start the vacuum pump and keep it working during the whole synthesis process.
Step 2: To close the valve I and open the valve II to pump the reaction tube to vacuum.
Step 3: To close the valve II and then open the valve I to introduce the working gas.
Step 4: To open the valve II and then adjust the two valves to keep the vacuum tube at a certain pressure.
Step 5: To introduce the carbon sources into the reaction area to start the deposition and pump out the exhaust gas.
3. Examples of the preparation of gas sensing materials based on graphene/ZrO2 composites
3.1 Example 1
Step 1: To place 2g ZrO2 particles with a diameter of 100nm into the reaction tube with a diameter of 20mm in the MPCVD device.
Step 2: To close the valve I and open the valve II to pump the reaction tube to a vacuum pressure of100mbar.
Step 3: To open the valve I and inject the working gas hydrogen with a flow rate of 150sccm. Then the methane as carbon source is introduced with a flow rate of sccm carried by argon with a flow rate of 135sccm. Keep the hydrogen flow rate constant.
Step 4: To turn on the power supply of the MPCVD device and start the reaction to deposit graphene on ZrO2 particles with a microwave power of 0.75kW and growth time of 30 minutes.
Step 5: After the reaction, the graphene/ZrO2 composites with a high specific surface area is obtained (Fig. 2).
3.2 Example 2
Step 1: To place 6g ZrO2 particles with a diameter of 75nm into the reaction tube with a diameter of 30mm in the MPCVD device.
Step 2: To close the valve I and open the valve II to pump the reaction tube to a vacuum pressure of 150mbar.
Step 3: To open the valve I and inject the working gas hydrogen with a flow rate of 130sccm. Then the ethylene as carbon source is introduced with a flow rate of sccm carried by argon with a flow rate of 140sccm. Keep the hydrogen flow rate constant.
Step 4: To turn on the power supply of the MPCVD device and start the reaction to deposit graphene on ZrO2 particles with a microwave power of 0.5kW and growth time of 60 minutes.
Step 5: After the reaction, the graphene/ZrO2 composites with a high specific surface area is obtained (Fig. 3).
1. The procedure of the preparation of gas sensing materials based on graphene/ZrO2 composites
Step 1: To place ZrO2 particles with a diameter of 50-100nm into the reaction tube in the Microwave Plasma Chemical Vapor Deposition (MPCVD) device.
Step 2: To control the vacuum chamber at a pressure of 100150mbar.
Step 3: To carry the carbon sources with a flow rate of 10-100sccm by the working gas with a flow rate of 100-200sccm, which is going to be hydrogen, argon or the mixture of both, into the area where the microwave plasma reaction occurs. The carbon sources described are going to be one or several kinds of organic compounds containing carbon atoms of SP 3 or SP 2 such as methane, methanol, ethanol or methyl formate.
Step 4: To turn on the power supply of the MPCVD device and start the reaction to deposit graphene on ZrO2 particles with a growth time of 5-60 minutes.
Step 5: After the reaction, the graphene/ZrO2 composites with a high specific surface area is obtained.
Step 6: To characterize the gas sensing properties of the synthesized graphene/ZrO2 composites.
2. The components of the Microwave Plasma Chemical Vapor Deposition system for preparing gas sensing materials based on graphene/ZrO2 composites are as follows:
A microwave source with a power range of 0.50-kW is used to provide the microwave plasma. A reaction tube with a diameter of 2050mm are arranged inside the microwave source as reaction and protective chamber. A gas inlet pipe and a gas outlet pipe are connected with each end of the reaction tube for the inlet and outlet of gas respectively. A vacuum pump is employed to pump out the gas inside the reaction tube. A barometer is connected to the gas inlet pipe to monitor the pressure inside the tube. Two valves (valve I and valve II, see Fig. 1) are connected to the gas inlet pipe and gas outlet pipe to control the gas in/out or not respectively.
3. The procedure of the control of two valves
Step 1: To start the vacuum pump and keep it working during the whole synthesis process.
Step 2: To close the valve I and open the valve II to pump the reaction tube to vacuum.
Step 3: To close the valve II and then open the valve I to introduce the working gas.
Step 4: To open the valve II and then adjust the two valves to keep the vacuum tube at a certain pressure.
Step 5: To introduce the carbon sources into the reaction area to start the deposition and pump out the exhaust gas.
Fig. 1 Schematic diagram of the MPCVD device
Fig. 2 Schematic diagram of the composite structure of graphene/SnO2
Fig. 3 SEM diagram of obtained graphene/SnO2 composites
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2812131C1 (en) * | 2023-03-28 | 2024-01-23 | Федеральное государственное бюджетное учреждение науки Институт металлургии и материаловедения им. А.А. Байкова Российской академии наук (ИМЕТ РАН) | Method for producing nanostructured powder composite based on graphene and zirconium dioxide using hexamethylenalnine |
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2021
- 2021-04-12 AU AU2021101870A patent/AU2021101870A4/en not_active Ceased
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2812131C1 (en) * | 2023-03-28 | 2024-01-23 | Федеральное государственное бюджетное учреждение науки Институт металлургии и материаловедения им. А.А. Байкова Российской академии наук (ИМЕТ РАН) | Method for producing nanostructured powder composite based on graphene and zirconium dioxide using hexamethylenalnine |
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