CN106556624A - A kind of preparation method of nanostructured gas sensitive - Google Patents
A kind of preparation method of nanostructured gas sensitive Download PDFInfo
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- CN106556624A CN106556624A CN201610889592.6A CN201610889592A CN106556624A CN 106556624 A CN106556624 A CN 106556624A CN 201610889592 A CN201610889592 A CN 201610889592A CN 106556624 A CN106556624 A CN 106556624A
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- gas
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- acetylene
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- G—PHYSICS
- 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
- 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
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
A kind of preparation method of nano indium oxide gas sensitive, belongs to oxide gas-sensing material field.The present invention is using chemical vapour deposition technique in In2O3Nano grain surface decomposes the In for preparing carbon coating by acetylene gas2O3Nano-particle, by the composition and pattern of annealing regulation and control surface carbon material, obtains nanometer In of the carbon modification that air-sensitive performance is significantly increased2O3Gas sensitive.Nanometer In that carbon is modified by the present invention first2O3Materials application is in gas detecting direction, relative to the method for other raising gas sensitive performances, such as sputtering or evaporation prepares metal oxide semiconductor films, sol-gal process and prepares the methods such as the nano-particle with special microstructure appearance, modification doped precious metal Pt, Pd, Au, the present invention has the advantages that method is simple, with low cost, and the In of the carbon modification for obtaining2O3The air-sensitive performance of gas-sensitive nano material increases significantly, and is with a wide range of applications in gas sensitive field.
Description
Technical field
The invention belongs to oxide gas-sensing material field, and in particular to a kind of In of carbon modification2O3The system of gas-sensitive nano material
Preparation Method.
Background technology
The gas sensitive adopted by present gas sensor is Metal oxide semiconductor gas-sensitiveness material mostly, its work
It is to react by conductor oxidate surface adsorption gas or with gas as principle and causes the change of semiconductor resistor
To detect a certain or several gases.As metal oxide semiconductor gas sensor has higher sensitivity, faster
Response recovery time, circuit and many merits such as simple to operate, cheap, and it is widely used medical treatment, aviation, house
The every field such as life, gas discharge detection.In2O3It is a kind of new gas sensitive, with SnO2、ZnO、Fe2O3In traditional gas
Quick material is compared, and which has the advantages that wider energy gap, less resistivity and higher catalysis activity.Therefore can lead to
Overload noble metal（Oxide）, donor-type or acceptor type energy level are formed, and so as to improve its air-sensitive performance, it are made for certain
Gas has higher sensitivity or selectivity.In2O3Gas sensitive may apply to flammable explosive gas, toxic and harmful
Leakage alarm, the field such as the monitor in real time of environmental quality.
China is the most abundant country of indium resource, and indium big producing country, but Shang Chu is probed in the deep processing to its high-tech
In the primary stage.In2O3The research of based nano-material is concentrated mainly on last decade, and also many problems need research.Therefore,
Explore high-performance In2O3Base functional material is a problem for still needing to solve.A kind of nanometer is disclosed in patent CN105424763A
The preparation method of tin dioxide gas-sensitive material, prepares the SnO of carbon coating using chemical vapour deposition technique2Nano-particle, but there is no
The method is applied to prepare the report of Indium sesquioxide..
The content of the invention
The invention provides a kind of In of carbon modification2O3The preparation method of gas-sensitive nano material, by high temperature induction acetylene gas
Body decomposes, and the carbon granule of generation is in In2O3Surface formation of deposits carbon-coating, is then made annealing treatment in an inert atmosphere, regulates and controls surface carbon
The composition and pattern of layer, finally gives the In of the enhanced carbon modification of air-sensitive performance2O3Gas-sensitive nano material.It is of the invention with it is existing
Metal oxide semiconductor gas-sensitiveness material preparation method is as prepared metal oxide semiconductor films, colloidal sol by sputtering or evaporation
Gel method prepares the nano-particle of special appearance, the modification method such as doped precious metal such as Pt, Pd, Au and compares, with process is simple,
The advantage of low cost, and In can be obviously improved2O3The air-sensitive performance of gas sensitive.
Technical scheme is as follows：
Methods described is with In2O3Powder and acetylene are raw material, by chemical vapour deposition technique in In2O3Powder surface passes through acetylene
Gas decomposes the In for preparing carbon coating2O3Powder of nanometric particles, by the In of the annealing regulation and control carbon coating2O3Receive
The composition and pattern of the surface carbon material of rice grain powder, obtains the nano indium oxide gas of the carbon modification that air-sensitive performance is significantly increased
Quick material.
Further, the preparation method is comprised the following steps：
Step 1：By In2O3Powder is placed in vacuum tube furnace, is warming up to 200～600 DEG C under an inert atmosphere, insulation 30～
60min；
Step 2：Keep electron tubes type in-furnace temperature constant, while being passed through the noble gases and stream that flow is 10～100mL/min
The acetylene gas for 20～150mL/min are measured, to the volume and In of the acetylene being passed through2O3Quality ratio be 20～3000mL/g
When, stopping is passed through acetylene, and maintains inert gas flow constant, is cooled to room temperature with the rate of temperature fall of 3～10 DEG C/min, obtains final product
To the In of carbon coating2O3Powder of nanometric particles；
Step 3：Carbon coating In that step 2 is obtained2O3Powder of nanometric particles is placed in vacuum tube furnace, under an inert atmosphere
300～800 DEG C of 1～12h of annealing, that is, obtain the nano indium oxide gas sensitive of carbon modification.
Further, wherein step 1 is warming up to 300 DEG C under an inert atmosphere, is incubated 30min.
Further, the wherein volume and In of the acetylene that step 2 is passed through2O3Quality ratio be 60mL/g.
Beneficial effects of the present invention are：The present invention is passed through second in high temperature environments by aumospheric pressure cvd method
Alkynes gas, using acetylene heat stability it is poor, be easily decomposed into carbon and hydrogen, and the carbon granule for generating is in In2O3Surface deposition obtains carbon
The In of cladding2O3Powder of nanometric particles, is then made annealing treatment under an inert atmosphere, obtains the nano indium oxide air-sensitive material of carbon modification
Material.With untreated In2O3Powder compares, and carbon of the present invention modifies nanometer In2O3The gas such as gas sensitive sensitivity, selectivity
Quick performance is significantly improved；Relative to other gas sensitive performance improvement methods, metal is prepared by sputtering or evaporation such as
Oxide semiconductor thin-film, sol-gal process prepare the nano material with special microstructure appearance, modification doped precious metal such as
The methods such as Pt, Pd, Au, the present invention have the advantages that process is simple, low cost, and the nano indium oxide air-sensitive of the carbon modification for obtaining
The air-sensitive performance of material is significantly increased, and is with a wide range of applications in gas sensitive field.
Specific embodiment
The present invention is done with reference to embodiment and further introduced.
A kind of preparation method of nano indium oxide gas sensitive, comprises the following steps：
Step 1：By In2O3Powder is evenly distributed in quartz boat, and is horizontally placed at vacuum tube furnace flat-temperature zone, is 10 in flow
Under the inert gas atmosphere of～100mL/min, with the heating rate of 3～10 DEG C/min by room temperature to 200～600 DEG C, protect
30～60min of temperature；
Step 2：Keep electron tubes type in-furnace temperature constant, while being passed through the noble gases and stream that flow is 10～100mL/min
The acetylene gas for 20～150mL/min are measured, the amount for being passed through acetylene gas is：Per 1g In2O3Correspondence is passed through 20～3000mL second
Alkynes；Then stop being passed through acetylene, and maintain inert gas flow constant, room temperature is cooled to the rate of temperature fall of 3～10 DEG C/min,
The In of carbon coating is obtained2O3Powder of nanometric particles；
Step 3：Carbon coating In that step 2 is obtained2O3Powder is put in quartz boat, is placed in vacuum tube furnace, in inertia
300～800 DEG C of 1～12h of annealing under gas shield, that is, obtain the nano indium oxide air-sensitive material of carbon modification of the present invention
Material；
Step 4：Nanometer In of the carbon modification that step 3 is obtained2O3Gas sensitive is coated on Al2O3Ceramic pipe surface, welding are drawn
Foot and heater strip make gas sensor, test its response to gas in room temperature within the temperature range of 500 DEG C；Wherein, survey
Gas testing body is ethanol, methane, acetylene, hydrogen etc..
Embodiment 1
A kind of preparation method of nano tin dioxide gas-sensitive material, comprises the following steps：
Step 1：Weigh 0.3g In2O3Powder is evenly distributed in quartz boat, and quartz boat is put into vacuum tube furnace flat-temperature zone,
The Ar gas of 30mL/min is passed through as protective gas, then with the speed of 5 DEG C/min by room temperature to 200 DEG C, insulation
30min；
Step 2：Keep 200 DEG C of electron tubes type in-furnace temperature constant, while being passed through acetylene gas and stream that flow is 30mL/min
The Ar oxygen mixtures for 60mL/min are measured, after 3min, stopping is passed through acetylene, and maintains the flow of Ar gas 60mL/min constant,
Room temperature is cooled to the rate of temperature fall of 3 DEG C/min, that is, obtains the In of carbon coating2O3Powder of nanometric particles；
Step 3：The In of the carbon coating that step 2 is obtained2O3Particle powder is placed in vacuum tube furnace after being put in quartz boat,
Flow is the lower 500 DEG C of annealing 2h of Ar protections of 60mL/min, that is, obtain the nano indium oxide air-sensitive material of carbon modification of the present invention
Material；
Step 4：Nanometer In of the carbon modification that step 3 is obtained2O3Gas sensitive is coated on Al2O3Ceramic pipe surface, welding pin
And heater strip makes gas sensor, its response to acetylene gas is tested within the temperature range of 500 DEG C in room temperature.
Embodiment 2
Tube furnace in 1 step 1 of embodiment is warming up to into 300 DEG C under Ar compression rings border, remaining operation is same as Example 1.
Embodiment 3
Tube furnace in 1 step 1 of embodiment is warming up to into 400 DEG C under Ar compression rings border, remaining operation is same as Example 1.
Embodiment 4
Tube furnace in 1 step 1 of embodiment is warming up to into 500 DEG C under Ar compression rings border, remaining operation is same as Example 1.
Embodiment 5
Tube furnace in 1 step 1 of embodiment is warming up to into 600 DEG C under Ar compression rings border, remaining operation is same as Example 1.
Embodiment 6
The time that acetylene gas are passed through in 3 step 2 of embodiment is adjusted to into 1min, remaining operation is same as Example 3.
Embodiment 7
The time that acetylene gas are passed through in 3 step 2 of embodiment is adjusted to into 5min, remaining operation is same as Example 3.
Embodiment 8
The time that acetylene gas are passed through in 3 step 2 of embodiment is adjusted to into 10min, remaining operation is same as Example 3.
Embodiment 9
The flow that acetylene gas are passed through in 3 step 2 of embodiment is adjusted to into 30mL/min, the flow for being passed through Ar gas is adjusted to
30mL/min, the time for being passed through C2H2 gases are adjusted to 3min, and remaining operation is same as Example 3.
Embodiment 10
The flow that acetylene gas are passed through in 3 step 2 of embodiment is adjusted to into 90mL/min, the flow for being passed through Ar gas is adjusted to
30mL/min, the time for being passed through acetylene gas are adjusted to 3min, and remaining operation is same as Example 3.
Claims (4)
1. a kind of preparation method of nano indium oxide gas sensitive, it is characterised in that methods described is with In2O3Powder and acetylene are
Raw material, by chemical vapour deposition technique in In2O3Decompose the In for preparing carbon coating by acetylene gas in powder surface2O3Receive
Rice grain powder, by the In of the annealing regulation and control carbon coating2O3The composition and shape of the surface carbon material of powder of nanometric particles
Looks, obtain the nano indium oxide gas sensitive of the carbon modification that air-sensitive performance is significantly increased.
2. preparation method as claimed in claim 1, it is characterised in that the preparation method is comprised the following steps：
Step 1：By In2O3Powder is placed in vacuum tube furnace, is warming up to 200～600 DEG C under an inert atmosphere, insulation 30～
60min；
Step 2：Keep electron tubes type in-furnace temperature constant, while being passed through the noble gases and stream that flow is 10～100mL/min
The acetylene gas for 20～150mL/min are measured, to the volume and In of the acetylene being passed through2O3Quality ratio be 20～3000mL/g
When, stopping is passed through acetylene, and maintains inert gas flow constant, is cooled to room temperature with the rate of temperature fall of 3～10 DEG C/min, obtains final product
To the In of carbon coating2O3Powder of nanometric particles；
Step 3：Carbon coating In that step 2 is obtained2O3Powder of nanometric particles is placed in vacuum tube furnace, and under an inert atmosphere 300
～800 DEG C of 1～12h of annealing, that is, obtain the nano indium oxide gas sensitive of carbon modification.
3. preparation method as claimed in claim 1, it is characterised in that：Wherein step 1 is warming up to 300 DEG C under an inert atmosphere,
Insulation 30min.
4. preparation method as claimed in claim 1, it is characterised in that：The wherein volume and In of the acetylene that step 2 is passed through2O3's
The ratio of quality is 60mL/g.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
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| CN2016106784100 | 2016-08-17 | ||
| CN201610678410 | 2016-08-17 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108918632A (en) * | 2018-06-29 | 2018-11-30 | 中国科学院合肥物质科学研究院 | A kind of the indium oxide nanosheet composite material preparation method and application of palladium nano-particles modification |
| CN109709184A (en) * | 2019-01-24 | 2019-05-03 | 吉林大学 | One kind being based on In2O3The NO of carbon dots compound2Sensor and preparation method thereof |
| CN110396408A (en) * | 2019-07-19 | 2019-11-01 | 电子科技大学 | A kind of preparation method of small particle YAG:Ce fluorescent powder |
| CN113252736A (en) * | 2021-05-07 | 2021-08-13 | 深圳技术大学 | Method for increasing gas selection function of multifunctional gas sensor and gas sensor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050100838A (en) * | 2004-04-16 | 2005-10-20 | 유일 | Indium oxide coated carbon |
| CN102623696A (en) * | 2012-03-31 | 2012-08-01 | 大连理工大学 | Preparation method for core-shell type carbon-coated iron nitride nano-composite particles and application of core-shell type carbon-coated iron nitride nano-composite particles |
| CN105424763A (en) * | 2015-10-30 | 2016-03-23 | 电子科技大学 | Preparation method of nanometer tin dioxide gas sensitive material |
-
2016
- 2016-10-12 CN CN201610889592.6A patent/CN106556624A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050100838A (en) * | 2004-04-16 | 2005-10-20 | 유일 | Indium oxide coated carbon |
| CN102623696A (en) * | 2012-03-31 | 2012-08-01 | 大连理工大学 | Preparation method for core-shell type carbon-coated iron nitride nano-composite particles and application of core-shell type carbon-coated iron nitride nano-composite particles |
| CN105424763A (en) * | 2015-10-30 | 2016-03-23 | 电子科技大学 | Preparation method of nanometer tin dioxide gas sensitive material |
Non-Patent Citations (2)
| Title |
|---|
| 张朝晖: "《检测技术及应用》", 30 November 2011, 中国质检出版社 * |
| 陈永: "《纳米材料制备与改性》", 31 July 2008, 万卷出版公司 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108918632A (en) * | 2018-06-29 | 2018-11-30 | 中国科学院合肥物质科学研究院 | A kind of the indium oxide nanosheet composite material preparation method and application of palladium nano-particles modification |
| CN108918632B (en) * | 2018-06-29 | 2020-05-29 | 中国科学院合肥物质科学研究院 | Preparation method and application of palladium nanoparticle modified indium oxide nanosheet composite material |
| CN109709184A (en) * | 2019-01-24 | 2019-05-03 | 吉林大学 | One kind being based on In2O3The NO of carbon dots compound2Sensor and preparation method thereof |
| CN109709184B (en) * | 2019-01-24 | 2020-12-01 | 吉林大学 | In-based2O3NO of carbon dot complexes2Sensor and preparation method thereof |
| CN110396408A (en) * | 2019-07-19 | 2019-11-01 | 电子科技大学 | A kind of preparation method of small particle YAG:Ce fluorescent powder |
| CN110396408B (en) * | 2019-07-19 | 2021-03-30 | 电子科技大学 | Preparation method of small-particle-size YAG (yttrium aluminum garnet) Ce fluorescent powder |
| CN113252736A (en) * | 2021-05-07 | 2021-08-13 | 深圳技术大学 | Method for increasing gas selection function of multifunctional gas sensor and gas sensor |
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Application publication date: 20170405 |