CN107128966A - Porous In2O3Ultrathin nanometer layer gas sensitive - Google Patents
Porous In2O3Ultrathin nanometer layer gas sensitive Download PDFInfo
- Publication number
- CN107128966A CN107128966A CN201710228006.8A CN201710228006A CN107128966A CN 107128966 A CN107128966 A CN 107128966A CN 201710228006 A CN201710228006 A CN 201710228006A CN 107128966 A CN107128966 A CN 107128966A
- Authority
- CN
- China
- Prior art keywords
- porous
- ultrathin nanometer
- nanometer layer
- gas sensitive
- layer gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- 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
-
- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
Abstract
The invention provides a kind of porous In2O3Ultrathin nanometer layer gas sensitive and its preparation and application.Described porous In2O3Ultrathin nanometer layer gas sensitive, with a cube crystalline phase, with porous ultrathin nanometer Rotating fields.Porous In2O3The pore size distribution of ultrathin nanometer layer gas sensitive is 0~85nm, In2O3Hole size on ultrathin nanometer layer is 2~4nm.Ultrathin nanometer thickness degree is 3.5~4nm, and specific surface area is 63~113m2/ g, can delicately detect the oxides of nitrogen gas in 10ppb~10ppm concentration ranges, response is 110~213 during detection 10ppm concentration oxides of nitrogen gas under 120 DEG C of operation temperatures.The present invention synthesizes the In with loose structure first under the conditions of template and surfactant is not introduced by simple two-step synthesis method2O3Ultrathin nanometer layer gas sensitive, the detection to oxides of nitrogen gas realizes relatively low operation temperature, extremely low detectable limit, high air-sensitive response, with important air-sensitive application value.
Description
Technical field
The invention belongs to gas sensing materials technical field, it is related to a kind of porous In2O3Ultrathin nanometer layer gas sensitive and its
Prepare and apply, and in particular to porous and two-dimensional ultrathin nano-layer structure square phase In2O3The preparation method of gas sensitive,
The material can delicately detect 10ppb~10ppm concentration range oxides of nitrogen gas.
Background technology
Nitrogen oxides is the general designation of nitric oxide and nitrogen dioxide gas, is that one kind is widely present in human being's production and life
In poisonous and contaminative gas.It is mainly derived from the by-product of the tail gas, industrial waste gas, commercial synthesis of vehicular emission
Thing etc..Therefore, develop the gas sensitive of highly sensitive stabilization to realize the real-time monitoring to oxides of nitrogen gas, be to ensure people
Healthy, environment-friendly and industry security the important subject of class (Science, 1971,173,45-47).
Metal oxide semiconductor is studied and most widely used gas sensitive.The resistance of metal oxide can be with
The change of ambient gas atmosphere and change, the monitoring to object gas is realized with this.In addition, metal oxide air-sensitive
Material also have the application advantage such as high sensitivity, low cost, high stability and portability (Angew.Chem.Int.Ed., 2010,
49,7632-7659).At present, there is diversified metal oxide (such as In2O3, ZnO, S nitrogen oxides etc.) be produced use
In detection oxides of nitrogen gas (Sens.Actuators, B, 2012,171,25-42).Property of the practical application for gas sensitive
Can there are many requirements, including high intensity, quick, stabilization response, and low detection temperature and detectable limit.
Develop inexpensive and high performance gas sensitive to meet the demand of practical application, be still extremely important and challenging
's.The performance of metal oxide gas sensitive is improved, can also be special by designing in addition to introducing expensive noble metal
Structure, pattern or interface.
Porous material has important air-sensitive application value, and being not only due to it has bigger serface, and pore passage structure
Be conducive to the transmission of gas.In numerous porous gas sensitives, metal oxide porous nano layer is due to having had porous knot concurrently
The advantage of structure and two-dimensional nano Rotating fields has obtained increasing research interest.Two-dimensional nano layer has bigger serface and can be sudden and violent
The particular crystal plane of dew, and then obtain substantial amounts of surface-active site.However, the non-laminar compound (Co of such as Emission in Cubic3O4With
In2O3) under chemical bond scission of link and growth tendency resistance, it is difficult to be built into two-dimensional nano Rotating fields.Therefore, construct with porous
The two-dimensional nano layer metal oxide of structure is more difficult, and is rarely reported.Li et al. reports the ZnO that thickness is 20~40nm
Porous nano layer gas sensitive is applied to acetone detection (J.Phys.Chem.C, 2010,114,14684-14691)；Sun et al.
It has studied air-sensitive property (CrystEngComm, 2011,13,3718- of thickness about 15nm S nitrogen oxides porous nano layer
3724)；The NiO porous nanos layer gas sensitive that Dong et al. develops micron order thickness is used to detect VOC
(RSC Adv., 2015,5,4880-4885).At present, porous ultrathin nanometer layer gold of the thickness less than 5nm is not still developed
Belong to oxide gas-sensing material.Although ultra-thin thickness can obtain more surface-active sites, more it is not easy to construct.This
It is due to that ultrathin nanometer layer has very high surface energy, easy accumulated growth is together.
The content of the invention
It is an object of the invention to provide a kind of In with loose structure and two-dimensional ultrathin nano-layer structure2O3Gas sensitive
And preparation method thereof, the material can delicately detect oxides of nitrogen gas.
In order to achieve the above object, the invention provides a kind of porous In2O3Ultrathin nanometer layer gas sensitive, its feature exists
In with porous ultrathin nanometer Rotating fields, the thickness of ultrathin nanometer layer is 3.5~4nm.
Further, described porous In2O3Ultrathin nanometer layer gas sensitive has cube crystalline phase.
Further, described porous In2O3Ultrathin nanometer layer gas sensitive can detect 10ppb under 120 DEG C of operation temperatures
~10ppm oxides of nitrogen gas.
Further, described porous In2O3Ultrathin nanometer layer gas sensitive, which has, to be formed between ultrathin nanometer Rotating fields
Hole and be distributed in In2O3Hole on ultrathin nanometer layer, porous In2O3The Size Distribution in the hole of ultrathin nanometer layer gas sensitive
For 0~85nm, In2O3Hole size on ultrathin nanometer layer is 2~4nm.
Further, described porous In2O3The thickness of the ultrathin nanometer layer of ultrathin nanometer layer gas sensitive for 3.5~
4nm。
Further, described porous In2O3The specific surface area of ultrathin nanometer layer gas sensitive is 63~113m2/g。
Further, described porous In2O3Ultrathin nanometer layer gas sensitive is under 120 DEG C of operation temperatures, to 10ppm nitrogen
The response of oxide is 110~213.
Present invention also offers above-mentioned porous In2O3The preparation method of ultrathin nanometer layer gas sensitive, it is characterised in that
Comprise the following steps：
Step 1：Indium glycerine salt is dispersed in deionized water, hydro-thermal reaction is carried out in a kettle., reaction is obtained
White solid centrifuge, cleaning and dry, obtain powder sample；
Step 2：The powder sample that step 1 is obtained calcination processing in atmosphere, that is, obtain porous In2O3Ultrathin nanometer layer
Gas sensitive.
Preferably, the ratio between volume of indium glycerine salt, the consumption of deionized water and reactor is 0.2 in described step 1
~0.4g: 30mL: 50mL.
Preferably, the reaction temperature of the hydro-thermal reaction described in step 1 is 50~70 DEG C, and the reaction time is 60~80min.
Preferably, calcination processing in the air described in step 2, reaction temperature is 300~500 DEG C, and the reaction time is 2h
~3h.
Present invention also offers above-mentioned porous In2O3Ultrathin nanometer layer gas sensitive is in detection oxides of nitrogen gas
Using.
The present invention utilizes simple two-step synthetic method, have developed the In with loose structure2O3Ultrathin nanometer layer air-sensitive
Material.The porous In2O3Ultrathin nanometer layer gas sensitive can delicately detect the nitrogen oxides of 10ppb~10ppm concentration ranges
Gas, with important application value.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention is synthesized first under the conditions of template and surfactant is not introduced by simple two-step synthesis method
In with loose structure2O3Ultrathin nanometer layer gas sensitive.The present invention realizes three simultaneously by simple two-step synthesis method
Highly difficult structure design：(1) by the In of non-laminar compound Emission in Cubic2O3It is built into two-dimensional layered structure；(2)In2O3Nanometer
The thickness of layer realizes 3.5~4nm ultra thin dimensions；(3) in In2O3Homogeneous meso-hole structure has been constructed on ultrathin nanometer layer.This hair
The porous In of bright exploitation2O3Ultrathin nanometer layer, with ultra-thin two-dimensional structure and loose structure, can delicately be detected very much
The oxides of nitrogen gas of 10ppb~10ppm concentration ranges, realizes relatively low detection temperature (120 DEG C), extremely low detectable limit
(10ppb), the response to 10ppm oxides of nitrogen gas under 120 DEG C of operation temperatures is up to 213, with important air-sensitive
Application value.
Brief description of the drawings
Fig. 1 is the porous In in embodiment 12O3The X-ray diffractogram of ultrathin nanometer layer gas sensitive, with PDF#06-0416
Standard card control is consistent.
Fig. 2 is the porous In in embodiment 12O3The stereoscan photograph of ultrathin nanometer layer gas sensitive.
Fig. 3 is the porous In in embodiment 12O3The atomic force microscopy of ultrathin nanometer layer gas sensitive.
Fig. 4 is the porous In in embodiment 12O3Nitrogen adsorption-desorption isotherm spectrogram of ultrathin nanometer layer gas sensitive.
Fig. 5 is the porous In in embodiment 12O3The pore size distribution curve figure of ultrathin nanometer layer gas sensitive.
Fig. 6 is the porous In in embodiment 12O3The transmission electron microscope photo of ultrathin nanometer layer gas sensitive, a transmits for low power
Electromicroscopic photograph, b~e is the high power transmission electron microscope photo of correspondence different zones in a photos.
Fig. 7 is the porous In in embodiment 12O3Ultrathin nanometer layer gas sensitive is circulated at a temperature of 120 DEG C is exposed to concentration
It is incremented by the response curve in the oxides of nitrogen gas of (10ppb~10ppm).
Embodiment
The preparation method of the indium glycerine salt used in various embodiments of the present invention with reference to document RSC Adv., and 2015,5,
5424-5431, specific method is：By 0.3g In (NO3)3·4.5H2O is dissolved into 30mL isopropanols, adds 10g the third three
Alcohol.Mixed system is transferred among 50mL ptfe autoclaves, 1h is heated at 180 DEG C.Naturally cool to after room temperature,
By solid precipitation and centrifugal separation, and respectively with deionized water and washes of absolute alcohol three times.12h is dried in 80 DEG C of baking ovens to produce
To indium glycerine salt.
Porous In in the present invention2O3Ultrathin nanometer layer gas sensitive loose structure be by nitrogen adsorption be desorbed test come
(the Micromeritics ASAP2010 series Full-automatic physicals chemical adsorption instrument) characterized：The characterization result of acquisition includes nitrogen
Adsorption/desorption isotherms, BET specific surface area and pore-size distribution.
Porous In2O3The air-sensitive performance of ultrathin nanometer layer gas sensitive is determined：
The test of air-sensitive performance is completed using CGS-8 gas sensings test device.I.e. by by porous In2O3Ultrathin nanometer
Layer gas sensitive is exposed in oxides of nitrogen gas atmosphere, detects the change of its resistance to detect its air-sensitive performance.Air-sensitive performance
Detection oxides of nitrogen gas used is nitrogen dioxide and nitric oxide mixed gas (bibliography without fixed proportion：
J.Mater.Chem.A, 2014,2,949-956；CrystEngComm, 2014,16,9116-9124), the preparation of nitrogen oxides
Method is：5g copper sheets are positioned in the concentrated nitric acid that 40mL mass concentrations are 65%, react at room temperature 5min, recycle air by nitrogen oxygen
Compound dilution obtains required concentration.Envionmental humidity~30%, operation temperature is 120 DEG C, the concentration of oxides of nitrogen gas
It is 10ppb~10ppm, the computational methods of response are S=(Rg-Ra)/Ra(Rg is gas sensitive in oxides of nitrogen gas
Resistance, RaIt is the aerial resistance of gas sensitive).
Embodiment 1
A kind of porous In2O3Ultrathin nanometer layer gas sensitive, its preparation method and air-sensitive performance are：
0.2g indium glycerine salt is dispersed in 30mL deionized waters, in 50mL ptfe autoclaves under the conditions of 50 DEG C
Middle hydro-thermal reaction 60min, the white solid that reaction is obtained is centrifuged, cleaned with deionized water, 60 DEG C of drying.By what is obtained
Powder sample calcines 2h for 400 DEG C in atmosphere, that is, obtains porous In2O3Ultrathin nanometer layer gas sensitive.
As shown in figure 1, the porous In of gained2O3The X-ray diffractogram of ultrathin nanometer layer gas sensitive, with PDF#06-0416
Standard card control is consistent.As a result show, the composition of the sample prepared is a cube crystalline phase In2O3, and crystallinity is good.
As shown in Fig. 2 the porous In of gained2O3The stereoscan photograph of ultrathin nanometer layer gas sensitive, as a result shows, makes
Standby obtained porous In2O3The pattern of ultrathin nanometer layer gas sensitive is dispersed porous ultrathin nanometer Rotating fields, porous
In2O3Ultrathin nanometer layer gas sensitive, which has, to be formed at the hole between ultrathin nanometer Rotating fields and is distributed in In2O3Ultrathin nanometer
Hole on layer.
As shown in figure 3, the porous In of gained2O3The atomic force microscopy of ultrathin nanometer layer gas sensitive, as a result table
Porous In that is bright, preparing2O3The nanometer layer thickness about 3.7nm of ultrathin nanometer layer gas sensitive.
As shown in figure 4, the porous In of gained2O3The nitrogen adsorption isotherm of ultrathin nanometer layer gas sensitive, as a result shows,
The porous In prepared2O3Ultrathin nanometer layer gas sensitive has loose structure, and its BET specific surface area is 92m2/g。
As shown in figure 5, the porous In of gained2O3The pore size distribution curve of ultrathin nanometer layer gas sensitive, as a result shows, makes
Standby obtained porous In2O3The pore size distribution of ultrathin nanometer layer gas sensitive is 0~85nm.
As shown in fig. 6, the porous In of gained2O3The transmission electron microscope photo of ultrathin nanometer layer gas sensitive, as a result shows, makes
Standby obtained porous In2O3The nanometer layer of ultrathin nanometer layer gas sensitive has homogeneous meso-hole structure, In2O3Ultrathin nanometer layer
On hole size be 2~4nm.
As shown in fig. 7, the porous In of gained2O3Ultrathin nanometer layer gas sensitive is circulated under 120 DEG C of operation temperatures to be exposed to
Response curve in the oxides of nitrogen gas of increasing concen-trations (10ppb~10ppm).As a result show, the porous In prepared2O3
Ultrathin nanometer layer gas sensitive can delicately detect the nitrogen oxygen in 10ppb~10ppm concentration ranges under 120 DEG C of operation temperatures
Compound gas, response is 213 during detection 10ppm concentration oxides of nitrogen gas.
Embodiment 2
A kind of porous In2O3Ultrathin nanometer layer gas sensitive, its preparation method and air-sensitive performance are：
0.3g indium glycerine salt is dispersed in 30mL deionized waters, in 50mL ptfe autoclaves under the conditions of 50 DEG C
Middle hydro-thermal reaction 60min, the white solid that reaction is obtained is centrifuged, cleaned with deionized water, 60 DEG C of drying.By what is obtained
Powder sample calcines 2h for 400 DEG C in atmosphere, that is, obtains porous In2O3Ultrathin nanometer layer gas sensitive.With a cube crystalline phase, it is
Dispersed porous ultrathin nanometer Rotating fields, ultrathin nanometer thickness degree about 3.7nm, described porous In2O3Ultrathin nanometer layer
Gas sensitive, which has, to be formed at the hole between ultrathin nanometer Rotating fields and is distributed in In2O3Hole on ultrathin nanometer layer, it is porous
In2O3The pore size distribution of ultrathin nanometer layer gas sensitive is 0~85nm, In2O3Hole size on ultrathin nanometer layer for 2~
4nm.BET specific surface area is 92m2/ g, can delicately be detected in 10ppb~10ppm concentration ranges under 120 DEG C of operation temperatures
Oxides of nitrogen gas, detection 10ppm concentration oxides of nitrogen gas when response be 213.
Embodiment 3
A kind of porous In2O3Ultrathin nanometer layer gas sensitive, its preparation method and air-sensitive performance are：
0.4g indium glycerine salt is dispersed in 30mL deionized waters, in 50mL ptfe autoclaves under the conditions of 50 DEG C
Middle hydro-thermal reaction 60min, the white solid that reaction is obtained is centrifuged, cleaned with deionized water, 60 DEG C of drying.By what is obtained
Powder sample calcines 2h for 400 DEG C in atmosphere, that is, obtains porous In2O3Ultrathin nanometer layer gas sensitive.With a cube crystalline phase, it is
Dispersed porous ultrathin nanometer Rotating fields, ultrathin nanometer thickness degree about 3.7nm, described porous In2O3Ultrathin nanometer layer
Gas sensitive, which has, to be formed at the hole between ultrathin nanometer Rotating fields and is distributed in In2O3Hole on ultrathin nanometer layer, it is porous
In2O3The pore size distribution of ultrathin nanometer layer gas sensitive is 0~85nm, In2O3Hole size on ultrathin nanometer layer for 2~
4nm.BET specific surface area is 92m2/ g, can delicately be detected in 10ppb~10ppm concentration ranges under 120 DEG C of operation temperatures
Oxides of nitrogen gas, detection 10ppm concentration oxides of nitrogen gas when response be 213.
Embodiment 4
A kind of porous In2O3Ultrathin nanometer layer gas sensitive, its preparation method and air-sensitive performance are：
0.2g indium glycerine salt is dispersed in 30mL deionized waters, in 50mL ptfe autoclaves under the conditions of 60 DEG C
Middle hydro-thermal reaction 60min, the white solid that reaction is obtained is centrifuged, cleaned with deionized water, 60 DEG C of drying.By what is obtained
Powder sample calcines 2h for 400 DEG C in atmosphere, that is, obtains porous In2O3Ultrathin nanometer layer gas sensitive.With a cube crystalline phase, it is
Dispersed porous ultrathin nanometer Rotating fields, ultrathin nanometer thickness degree about 3.7nm, described porous In2O3Ultrathin nanometer layer
Gas sensitive, which has, to be formed at the hole between ultrathin nanometer Rotating fields and is distributed in In2O3Hole on ultrathin nanometer layer, it is porous
In2O3The pore size distribution of ultrathin nanometer layer gas sensitive is 0~85nm, In2O3Hole size on ultrathin nanometer layer for 2~
4nm.BET specific surface area is 92m2/ g, can delicately be detected in 10ppb~10ppm concentration ranges under 120 DEG C of operation temperatures
Oxides of nitrogen gas, detection 10ppm concentration oxides of nitrogen gas when response be 213.
Embodiment 5
A kind of porous In2O3Ultrathin nanometer layer gas sensitive, its preparation method and air-sensitive performance are：
0.2g indium glycerine salt is dispersed in 30mL deionized waters, in 50mL ptfe autoclaves under the conditions of 70 DEG C
Middle hydro-thermal reaction 60min, the white solid that reaction is obtained is centrifuged, cleaned with deionized water, 60 DEG C of drying.By what is obtained
Powder sample calcines 2h for 400 DEG C in atmosphere, that is, obtains porous In2O3Ultrathin nanometer layer gas sensitive.With a cube crystalline phase, it is
Dispersed porous ultrathin nanometer Rotating fields, ultrathin nanometer thickness degree about 3.7nm, described porous In2O3Ultrathin nanometer layer
Gas sensitive, which has, to be formed at the hole between ultrathin nanometer Rotating fields and is distributed in In2O3Hole on ultrathin nanometer layer, it is porous
In2O3The pore size distribution of ultrathin nanometer layer gas sensitive is 0~85nm, In2O3Hole size on ultrathin nanometer layer for 2~
4nm.BET specific surface area is 92m2/ g, can delicately be detected in 10ppb~10ppm concentration ranges under 120 DEG C of operation temperatures
Oxides of nitrogen gas, detection 10ppm concentration oxides of nitrogen gas when response be 213.
Embodiment 6
A kind of porous In2O3Ultrathin nanometer layer gas sensitive, its preparation method and air-sensitive performance are：
0.2g indium glycerine salt is dispersed in 30mL deionized waters, in 50mL ptfe autoclaves under the conditions of 50 DEG C
Middle hydro-thermal reaction 70min, the white solid that reaction is obtained is centrifuged, cleaned with deionized water, 60 DEG C of drying.By what is obtained
Powder sample calcines 2h for 400 DEG C in atmosphere, that is, obtains porous In2O3Ultrathin nanometer layer gas sensitive.With a cube crystalline phase, it is
Dispersed porous ultrathin nanometer Rotating fields, ultrathin nanometer thickness degree about 3.7nm, described porous In2O3Ultrathin nanometer layer
Gas sensitive, which has, to be formed at the hole between ultrathin nanometer Rotating fields and is distributed in In2O3Hole on ultrathin nanometer layer, it is porous
In2O3The pore size distribution of ultrathin nanometer layer gas sensitive is 0~85nm, In2O3Hole size on ultrathin nanometer layer for 2~
4nm.BET specific surface area is 92m2/ g, can delicately be detected in 10ppb~10ppm concentration ranges under 120 DEG C of operation temperatures
Oxides of nitrogen gas, detection 10ppm concentration oxides of nitrogen gas when response be 213.
Embodiment 7
A kind of porous In2O3Ultrathin nanometer layer gas sensitive, its preparation method and air-sensitive performance are：
0.2g indium glycerine salt is dispersed in 30mL deionized waters, in 50mL ptfe autoclaves under the conditions of 50 DEG C
Middle hydro-thermal reaction 80min, the white solid that reaction is obtained is centrifuged, cleaned with deionized water, 60 DEG C of drying.By what is obtained
Powder sample calcines 2h for 400 DEG C in atmosphere, that is, obtains porous In2O3Ultrathin nanometer layer gas sensitive.With a cube crystalline phase, it is
Dispersed porous ultrathin nanometer Rotating fields, ultrathin nanometer thickness degree about 3.7nm, described porous In2O3Ultrathin nanometer layer
Gas sensitive, which has, to be formed at the hole between ultrathin nanometer Rotating fields and is distributed in In2O3Hole on ultrathin nanometer layer, it is porous
In2O3The pore size distribution of ultrathin nanometer layer gas sensitive is 0~85nm, In2O3Hole size on ultrathin nanometer layer for 2~
4nm.BET specific surface area is 92m2/ g, can delicately be detected in 10ppb~10ppm concentration ranges under 120 DEG C of operation temperatures
Oxides of nitrogen gas, detection 10ppm concentration oxides of nitrogen gas when response be 213.
Embodiment 8
A kind of porous In2O3Ultrathin nanometer layer gas sensitive, its preparation method and air-sensitive performance are：
0.2g indium glycerine salt is dispersed in 30mL deionized waters, in 50mL ptfe autoclaves under the conditions of 50 DEG C
Middle hydro-thermal reaction 60min, the white solid that reaction is obtained is centrifuged, cleaned with deionized water, 60 DEG C of drying.By what is obtained
Powder sample calcines 2h for 300 DEG C in atmosphere, that is, obtains porous In2O3Ultrathin nanometer layer gas sensitive.With a cube crystalline phase, it is
Dispersed porous ultrathin nanometer Rotating fields, ultrathin nanometer thickness degree about 3.5nm, described porous In2O3Ultrathin nanometer layer
Gas sensitive, which has, to be formed at the hole between ultrathin nanometer Rotating fields and is distributed in In2O3Hole on ultrathin nanometer layer, it is porous
In2O3The pore size distribution of ultrathin nanometer layer gas sensitive is 0~85nm, In2O3Hole size on ultrathin nanometer layer for 2~
4nm.BET specific surface area is 113m2/ g, can delicately detect 10ppb~10ppm concentration ranges under 120 DEG C of operation temperatures
Interior oxides of nitrogen gas, response is 130 during detection 10ppm concentration oxides of nitrogen gas.
Embodiment 9
A kind of porous In2O3Ultrathin nanometer layer gas sensitive, its preparation method and air-sensitive performance are：
0.2g indium glycerine salt is dispersed in 30mL deionized waters, in 50mL ptfe autoclaves under the conditions of 50 DEG C
Middle hydro-thermal reaction 60min, the white solid that reaction is obtained is centrifuged, cleaned with deionized water, 60 DEG C of drying.By what is obtained
Powder sample calcines 2h for 500 DEG C in atmosphere, that is, obtains porous In2O3Ultrathin nanometer layer gas sensitive.With a cube crystalline phase, it is
Dispersed porous ultrathin nanometer Rotating fields, ultrathin nanometer thickness degree about 4.0nm, described porous In2O3Ultrathin nanometer layer
Gas sensitive, which has, to be formed at the hole between ultrathin nanometer Rotating fields and is distributed in In2O3Hole on ultrathin nanometer layer, it is porous
In2O3The pore size distribution of ultrathin nanometer layer gas sensitive is 0~85nm, In2O3Hole size on ultrathin nanometer layer for 2~
4nm.BET specific surface area is 63m2/ g, can delicately be detected in 10ppb~10ppm concentration ranges under 120 DEG C of operation temperatures
Oxides of nitrogen gas, detection 10ppm concentration oxides of nitrogen gas when response be 110.
Embodiment 10
A kind of porous In2O3Ultrathin nanometer layer gas sensitive, its preparation method and air-sensitive performance are：
0.2g indium glycerine salt is dispersed in 30mL deionized waters, in 50mL ptfe autoclaves under the conditions of 50 DEG C
Middle hydro-thermal reaction 60min, the white solid that reaction is obtained is centrifuged, cleaned with deionized water, 60 DEG C of drying.By what is obtained
Powder sample calcines 2.5h for 400 DEG C in atmosphere, that is, obtains porous In2O3Ultrathin nanometer layer gas sensitive.With a cube crystalline phase,
For dispersed porous ultrathin nanometer Rotating fields, ultrathin nanometer thickness degree about 3.7nm, described porous In2O3Ultrathin nanometer
Layer gas sensitive, which has, to be formed at the hole between ultrathin nanometer Rotating fields and is distributed in In2O3Hole on ultrathin nanometer layer, it is porous
In2O3The pore size distribution of ultrathin nanometer layer gas sensitive is 0~85nm, In2O3Hole size on ultrathin nanometer layer for 2~
4nm.BET specific surface area is 90m2/ g, can delicately be detected in 10ppb~10ppm concentration ranges under 120 DEG C of operation temperatures
Oxides of nitrogen gas, detection 10ppm concentration oxides of nitrogen gas when response be 210.
Embodiment 11
A kind of porous In2O3Ultrathin nanometer layer gas sensitive, its preparation method and air-sensitive performance are：
0.2g indium glycerine salt is dispersed in 30mL deionized waters, in 50mL ptfe autoclaves under the conditions of 50 DEG C
Middle hydro-thermal reaction 60min, the white solid that reaction is obtained is centrifuged, cleaned with deionized water, 60 DEG C of drying.By what is obtained
Powder sample calcines 3h for 400 DEG C in atmosphere, that is, obtains porous In2O3Ultrathin nanometer layer gas sensitive.With a cube crystalline phase, it is
Dispersed porous ultrathin nanometer Rotating fields, ultrathin nanometer thickness degree about 3.8nm, described porous In2O3Ultrathin nanometer layer
Gas sensitive, which has, to be formed at the hole between ultrathin nanometer Rotating fields and is distributed in In2O3Hole on ultrathin nanometer layer, it is porous
In2O3The pore size distribution of ultrathin nanometer layer gas sensitive is 0~85nm, In2O3Hole size on ultrathin nanometer layer for 2~
4nm.BET specific surface area is 90m2/ g, can delicately be detected in 10ppb~10ppm concentration ranges under 120 DEG C of operation temperatures
Oxides of nitrogen gas, detection 10ppm concentration oxides of nitrogen gas when response be 210.
Comparative example 1
0.2g indium glycerine salt is dispersed in 30mL deionized waters, in 50mL ptfe autoclaves under the conditions of 50 DEG C
Middle hydro-thermal reaction 60min, the white solid that reaction is obtained is centrifuged, cleaned with deionized water, 60 DEG C of drying.By what is obtained
Powder sample calcines 2h for 600 DEG C in atmosphere, that is, obtains porous In2O3.With a cube crystalline phase, pattern is a small amount of nanometer layer fragment
With the mixing of nano-particle, loose structure, 0~120nm of aperture, BET specific surface area is 48m2/ g, under 120 DEG C of operation temperatures
The oxides of nitrogen gas in 10ppb~10ppm concentration ranges can be delicately detected, 10ppm concentration oxides of nitrogen gas is detected
When response be 72.
Comparative example 2
By 0.2g indium glycerine salt directly in atmosphere 400 DEG C of calcining 2h, porous In is obtained2O3Ball.With a cube crystalline phase,
Loose structure, pattern is medicine ball, and ball size is 450nm, and the pore-size distribution of loose structure is in 0~120nm, BET specific surface area
For 23m2/ g, can detect the oxides of nitrogen gas in 10ppb~10ppm concentration ranges under 120 DEG C of operation temperatures, detection
Response is 45 during 10ppm oxides of nitrogen gas.
Claims (10)
1. a kind of porous In2O3Ultrathin nanometer layer gas sensitive, it is characterised in that ultra-thin with porous ultrathin nanometer Rotating fields
The thickness of nanometer layer is 3.5~4nm.
2. porous In as claimed in claim 12O3Ultrathin nanometer layer gas sensitive, it is characterised in that with a cube crystalline phase.
3. porous In as claimed in claim 12O3Ultrathin nanometer layer gas sensitive, it is characterised in that described porous In2O3It is super
Thin nanometer layer gas sensitive, which has, to be formed at the hole between ultrathin nanometer Rotating fields and is distributed in In2O3On ultrathin nanometer layer
Hole, wherein, porous In2O3The Size Distribution in the hole of ultrathin nanometer layer gas sensitive is 0~85nm, In2O3On ultrathin nanometer layer
Hole size is 2~4nm.
4. porous In as claimed in claim 12O3Ultrathin nanometer layer gas sensitive, it is characterised in that specific surface area be 63~
113m2/g。
5. porous In as claimed in claim 12O3Ultrathin nanometer layer gas sensitive, it is characterised in that in 120 DEG C of operation temperatures
Lower to detect 10ppb~10ppm oxides of nitrogen gas, the nitrogen oxides response to 10ppm is 110~213.
6. the porous In any one of claim 1-52O3The preparation method of ultrathin nanometer layer gas sensitive, its feature exists
In comprising the following steps：
Step 1：Indium glycerine salt is dispersed in deionized water, hydro-thermal reaction is carried out in a kettle., by react obtain it is white
Color solid is centrifuged, cleans and dried, and obtains powder sample；
Step 2：The powder sample that step 1 is obtained calcination processing in atmosphere, that is, obtain porous In2O3Ultrathin nanometer layer air-sensitive
Material.
7. porous In as claimed in claim 62O3The preparation method of ultrathin nanometer layer gas sensitive, it is characterised in that step 1
The ratio between volume of middle indium glycerine salt, the consumption of deionized water and reactor is 0.2~0.4g: 30mL: 50mL.
8. porous In as claimed in claim 62O3The preparation method of ultrathin nanometer layer gas sensitive, it is characterised in that step 1
Described in the reaction temperature of hydro-thermal reaction be 50~70 DEG C, the reaction time is 60~80min.
9. porous In as claimed in claim 62O3The preparation method of ultrathin nanometer layer gas sensitive, it is characterised in that step 2
Described in air in calcination processing, reaction temperature is 300~500 DEG C, the reaction time be 2h~3h.
10. the porous In any one of claim 1-52O3Ultrathin nanometer layer gas sensitive is in detection oxides of nitrogen gas
In application.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710228006.8A CN107128966A (en) | 2017-06-09 | 2017-06-09 | Porous In2O3Ultrathin nanometer layer gas sensitive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710228006.8A CN107128966A (en) | 2017-06-09 | 2017-06-09 | Porous In2O3Ultrathin nanometer layer gas sensitive |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107128966A true CN107128966A (en) | 2017-09-05 |
Family
ID=59716269
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710228006.8A Pending CN107128966A (en) | 2017-06-09 | 2017-06-09 | Porous In2O3Ultrathin nanometer layer gas sensitive |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107128966A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111812161A (en) * | 2020-04-27 | 2020-10-23 | 清华大学 | NO based on metal oxide2Gas sensor and preparation method thereof |
| CN113686928A (en) * | 2021-08-24 | 2021-11-23 | 华北电力大学 | GO/In2O3Composite nano material and preparation and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1663914A (en) * | 2004-03-05 | 2005-09-07 | 中国科学院固体物理研究所 | Indium oxide film material and its preparation method |
| CN102001698A (en) * | 2010-10-26 | 2011-04-06 | 江苏大学 | Preparation method of indium oxide mesoporous nanospheres |
-
2017
- 2017-06-09 CN CN201710228006.8A patent/CN107128966A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1663914A (en) * | 2004-03-05 | 2005-09-07 | 中国科学院固体物理研究所 | Indium oxide film material and its preparation method |
| CN102001698A (en) * | 2010-10-26 | 2011-04-06 | 江苏大学 | Preparation method of indium oxide mesoporous nanospheres |
Non-Patent Citations (2)
| Title |
|---|
| XUE WANG ET AL.: ""Ultrathin In2O3 Nanosheets with Uniform Mesopores for Highly Sensitive Nitric Oxide Detection"", 《ACS APPLIED MATERIALS & INTERFACES》 * |
| YANG CAO ET AL.: ""Synthesis of porous In2O3 microspheres"", 《RSC ADV.》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111812161A (en) * | 2020-04-27 | 2020-10-23 | 清华大学 | NO based on metal oxide2Gas sensor and preparation method thereof |
| CN113686928A (en) * | 2021-08-24 | 2021-11-23 | 华北电力大学 | GO/In2O3Composite nano material and preparation and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Wang et al. | Au-loaded mesoporous WO3: preparation and n-butanol sensing performances | |
| Wang et al. | Rational shape control of porous Co3O4 assemblies derived from MOF and their structural effects on n-butanol sensing | |
| Song et al. | Preparation of biomorphic porous LaFeO3 by sorghum straw biotemplate method and its acetone sensing properties | |
| Wei et al. | Facile synthesis of La-doped In2O3 hollow microspheres and enhanced hydrogen sulfide sensing characteristics | |
| Qin et al. | Three-dimensionally ordered macroporous La1− xMgxFeO3 as high performance gas sensor to methanol | |
| Prim et al. | A novel mesoporous CaO‐loaded In2O3 material for CO2 sensing | |
| Li et al. | Preparation and characteristics of nanocrystalline NiO by organic solvent method | |
| Sangsefidi et al. | Synthesis, characterization and investigation of the electrochemical hydrogen storage properties of CuO–CeO2 nanocomposites synthesized by green method | |
| Wang et al. | Structural and electronic engineering of 3DOM WO 3 by alkali metal doping for improved NO 2 sensing performance | |
| Gu et al. | Controlled synthesis of porous Ni-doped SnO2 microstructures and their enhanced gas sensing properties | |
| Feng et al. | Morphology-controlled synthesis of ZnSnO3 hollow spheres and their n-butanol gas-sensing performance | |
| Costa et al. | On the use of NiO as sintering additive for BaCe0, 9Y0, 1O3− α | |
| Zhao et al. | Preparation, characterization and catalytic application of hierarchically porous LaFeO 3 from a pomelo peel template | |
| Yan et al. | Synthesis and gas sensing application of porous CeO2–ZnO hollow fibers using cotton as biotemplates | |
| Dong et al. | Fabrication and formaldehyde sensing performance of Fe-doped In 2 O 3 hollow microspheres via a one-pot method | |
| Guo | Design of gas sensor based on Fe-doped ZnO nanosheet-spheres for low concentration of formaldehyde detection | |
| Pilliadugula et al. | Gas sensing performance of GaOOH and β-Ga2O3 synthesized by hydrothermal method: A comparison | |
| CN107128966A (en) | Porous In2O3Ultrathin nanometer layer gas sensitive | |
| CN107572579B (en) | A kind of spherical zinc oxide gas sensing material and preparation method thereof of bismuth doping | |
| Zhang et al. | Synthesis and NO 2 gas-sensing properties of coral-like indium oxide via a facile solvothermal method | |
| Biswas et al. | Studies on the sensing behaviour of nanocrystalline CuGa2O4 towards hydrogen, liquefied petroleum gas and ammonia | |
| Ortiz-Landeros et al. | Li2SiO3 fast microwave-assisted hydrothermal synthesis and evaluation of its water vapor and CO2 absorption properties | |
| Liu et al. | Template-free preparation of mesoporous single crystal In 2 O 3 achieving superior ethanol gas sensing performance | |
| Jing et al. | Co-doped LaFeO3 gas sensor for fast low-power acetone detection | |
| Liu et al. | In situ synthesis of Zn-doped In2S3/In2O3 composites for the monitoring of trace ethanol at low temperature |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170905 |