CN110386620A - Indium oxide gas sensitive and preparation method and application for ppb grades of ethyl alcohol detections - Google Patents
Indium oxide gas sensitive and preparation method and application for ppb grades of ethyl alcohol detections Download PDFInfo
- Publication number
- CN110386620A CN110386620A CN201910705271.XA CN201910705271A CN110386620A CN 110386620 A CN110386620 A CN 110386620A CN 201910705271 A CN201910705271 A CN 201910705271A CN 110386620 A CN110386620 A CN 110386620A
- Authority
- CN
- China
- Prior art keywords
- indium oxide
- ethyl alcohol
- detection
- gas
- nano
- 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
-
- 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
-
- 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
-
- 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
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Physics & Mathematics (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Immunology (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pathology (AREA)
- Inorganic Chemistry (AREA)
- Biochemistry (AREA)
- Electrochemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The present invention relates to a kind of indium oxide gas sensitives and preparation method and application for ppb grades of ethyl alcohol detections, belong to field of new materials.The present invention is prepared for nano-sheet indium oxide on the basis of improving the production method of indium oxide, using one step hydro thermal method.Indium oxide nanometer sheet is evenly distributed, and particle is smaller, is conducive to come into full contact with under test gas, expands specific surface area.Compared to traditional oxidation phosphide material, the more than one order of magnitude is improved to the response of ethyl alcohol, and ppb grades of ethyl alcohol of measurement may be implemented, lowest detection lower limit is 5ppb.Synthesizer of the present invention is simple, and strong operability, preparation condition is mild, reaction process cleanliness without any pollution, reproducible, realizes the highly selective and highly sensitive detection to alcohol gas, has great application prospect in ethyl alcohol detection field.
Description
Technical field
The present invention relates to a kind of indium oxide gas sensitives and preparation method and application for ppb grades of ethyl alcohol detections, belong to
Field of new materials.
Background technique
With the continuous development promoted with automobile industry of people's living standard, car ownership is continuously increased, driver
Traffic accident caused by driving when intoxicated also is increasing, and seriously threatens the safety of life and property of people.Therefore in order to avoid
Traffic accident caused by driving when intoxicated, needs to carry out driver's cabin the detection of real-time concentration of alcohol.Simultaneously in food processing, wine
The industries such as wine need to monitor concentration of alcohol in air.Therefore, the detection of concentration of alcohol is necessary.
Metal oxide semiconductor nano-material is widely used in air-sensitive research, but metal oxygen due to its unique advantage
The problem of generally existing sensitivity of compound material is low, poor selectivity, such as α-Fe2O3The N-shaped for being 2.1eV as a kind of band gap width
Semiconductor is commonly used to detection liquefied petroleum gas, alcohol gas, acetone gas, hydrogen sulfide gas, but its sensitivity is low, and exists
The problem of cross sensitivity.And CuO and NiO is commonly used to detection hydrogen sulfide gas, ammonia, titanium dioxide nitrogen as P-type semiconductor
The problem of body, formaldehyde gas etc., it is low similarly to there is sensitivity, poor selectivity.In recent years, in order to improve its sensitivity and selection
Property, people are made that unremitting effort, including precious metal doping Au, Ag, Pt, Pd, Cd etc. and Morphological control, nanometer
Grain, core-shell nanospheres, nano stick, nanotube, nanobelt and porous network etc..These inventions are improving metal oxide
It is made some progress in the sensitivity of gas sensitive.
The present invention uses one step hydro thermal method to be prepared for, and a kind of preparation process is simple and easy to control, and test result is shown compared to routine
Indium oxide significantly improves the sensitivity to ethyl alcohol, has reached 52 to the response of the alcohol gas of 50ppb, and selectivity is excellent, and
And the concentration of alcohol of 5ppb can be measured, this is the minimum concentration of alcohol that current oxidation phosphide material can measure.
Summary of the invention
The present invention provides a kind of indium oxide gas sensitive and preparation method and application for ppb grades of ethyl alcohol detections.This hair
Bright another to be solved technical problem is to provide a kind of purposes of above-mentioned functional material, using realization indium oxide to low concentration second
The high sensitivity of alcohol gas and highly selective detection.
A kind of nano indium oxide gas sensitive for the detection of ppb grades of ethyl alcohol, the pattern of the indium oxide functional material are
The material of laminated structure, the granular size of nanometer sheet are 20~100nm.
It is a further object of the present invention to provide the preparation methods of nano indium oxide functional material.
A kind of preparation method of the nano indium oxide gas sensitive for the detection of ppb grades of ethyl alcohol, including following processing steps:
It is in molar ratio that 1:1~2:3~5 are dissolved in deionized water and are made by indium salts, cetrimonium and sodium hydroxide
Metal salt solution, the concentration of indium salts is 0.06~0.08mol/L in the metal salt solution；40~60min is persistently stirred, is allowed to
It is completely dissolved uniformly mixed；Obtained salting liquid is transferred in autoclave again, it is cooling after 160 DEG C of 18~20h of reaction
To precipitating；Finally gained is precipitated through centrifugation, washing, is dried to obtain hydroxide powder, in 350~400 DEG C of 2~3h of calcining
Obtain nano indium oxide functional material.
Preferably, the indium salts are inidum chloride or five water indium nitrates.
Preferably, the revolving speed when centrifugal treating is 4000~8000r/min, and each centrifugation time is 5~10 minutes.
Preferably, the carrying out washing treatment is successively to be washed 3~5 times using ethyl alcohol and deionized water.
Preferably, described to be dried as 10~20h dry at 60 DEG C.
Preferably, 3~5 DEG C/min of heating rate of the calcining, temperature rises to 350~400 DEG C of 2~3h of holding, in sky
Naturally it is cooled to room temperature in gas.
It is yet another object of the invention to provide the application of above-mentioned nano indium oxide functional material, the nano indium oxide function
Gas sensitive of the material as gas sensor, the detection for low-concentration ethanol gas.
The invention has the advantages that
The present invention is prepared for nanocube on the basis of improving the production method of indium oxide, using one step hydro thermal method
Indium oxide.Indium oxide nano cubic block is evenly distributed, and particle is smaller, is conducive to come into full contact with under test gas, expands specific surface
Product.Compared to traditional oxidation phosphide material, the more than one order of magnitude is improved to the response of ethyl alcohol, and ethyl alcohol may be implemented
Ppb grades of measurement, lowest detection lower limit are 5ppb.Synthesizer of the present invention is simple, and strong operability, preparation condition is mild,
Reaction process cleanliness without any pollution, it is reproducible, the highly selective and highly sensitive detection to alcohol gas is realized, is examined in ethyl alcohol
Survey field has great application prospect.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of nano indium oxide.
Fig. 2 is the transmission electron microscope picture of nano indium oxide.
Fig. 3 is the X-ray diffraction pattern of material of the present invention.
Fig. 4 be 1 products therefrom of embodiment at 270 DEG C of optimum working temperature to the toluene of 500ppb, benzene, formaldehyde, formic acid,
The response sensitivity histogram of the gases such as acetone, ammonia, ethyl alcohol.
Fig. 5 is the sensitivity characteristic curve graph one of material of the present invention measured.
Fig. 6 is the sensitivity characteristic curve graph two of material of the present invention measured.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.
Test method described in following embodiments is unless otherwise specified conventional method；The reagent and material, such as
Without specified otherwise, commercially obtain.
Embodiment 1
The present embodiment prepares nano indium oxide functional material, and the nano-functional material is laminated structure, the material
Preparation method includes hydro-thermal method and calcination method, and steps are as follows for specific completion:
Step 1, by 4mmol ln2O3·5H2O, 4mmol cetyl trimethylammonium bromide and 14mmol NaOH are dissolved in
It in 50mL deionized water, is sufficiently stirred and makes it completely dissolved, obtained uniform solution is transferred in polytetrafluoroethylene (PTFE) after 40min
In the stainless steel cauldron of lining, it is placed in 160 DEG C of baking oven and reacts 19h.
Step 2, at the end of to above-mentioned reaction, cooled to room temperature, by products therefrom water and ethyl alcohol centrifuge washing each 4
Secondary, revolving speed when centrifugal treating is 8000r/min, and then 60 DEG C of dry 10h are to obtain the predecessor of white color in an oven.
Step 3, by predecessor obtained in step 2 in air at 400 DEG C calcine 2h after (4 DEG C of heating rate/
Min), it is cooled to room temperature to get target product nano indium oxide functional material is arrived.
Embodiment 2
The present embodiment prepares nano indium oxide functional material, and the nano-functional material is cube structure, the material
Preparation method include hydro-thermal method and calcination method, it is specific to complete that steps are as follows:
Step 1, by 4mmol ln2O3·5H2O, 5mmol cetyl trimethylammonium bromide and 15mmol NaOH are dissolved in
It in 60mL deionized water, is sufficiently stirred and makes it completely dissolved, obtained uniform solution is transferred in polytetrafluoroethylene (PTFE) after 40min
In the stainless steel cauldron of lining, it is placed in 160 DEG C of baking oven and reacts 20h.
Step 2, at the end of to above-mentioned reaction, cooled to room temperature, by products therefrom water and ethyl alcohol centrifuge washing each 4
Secondary, revolving speed when centrifugal treating is 8000r/min, and then 60 DEG C of dry 10h are to obtain the predecessor of white color in an oven.
Step 3, by predecessor obtained in step 2 in air at 450 DEG C calcine 2h after (4 DEG C of heating rate/
Min), it is cooled to room temperature to get target product nano indium oxide functional material is arrived.
Resulting nano indium oxide functional material 1mL dehydrated alcohol is dispersed, measures 5~10 μ L indium oxides with liquid-transfering gun
The suspension of functional material, coating is to ceramic pipe surface, and the constantly rotating welding sensor base of ceramic tube, until target
Product uniformly coats until ceramic pipe surface.
The sensor for being coated with nano indium oxide functional material is placed in gas chamber, is heated to 200 DEG C, will after aging 1h
Under test gas is passed through gas chamber, reaction a period of time, is passed through air under test gas and drives gas chamber out of, by being passed through gas front and back material
Curent change realizes the detection to gas sensitivity.
Fig. 1 is the scanning electron microscope (SEM) photograph of nano indium oxide.
Fig. 2 is the transmission electron microscope picture of nano indium oxide.It can be clearly seen that the pattern of indium oxide in thin slice knot from figure
Structure, granular size are 20~100nm.
Fig. 3 is the X-ray diffraction pattern of material of the present invention, the position of You Tuzhong diffraction maximum and intensity and lattice fringe spacing
It can determine that this material is indium oxide.
Fig. 4 be 1 products therefrom of embodiment at 270 DEG C of optimum working temperature to the toluene of 500ppb, benzene, formaldehyde, formic acid,
The response sensitivity histogram of the gases such as acetone, ammonia, ethyl alcohol, as seen from the figure, 1 products therefrom of embodiment is to alcohol gas
There is extremely strong selectivity.It can be seen that 1 gained composite material of embodiment is realized to the highly selective and highly sensitive of alcohol gas
Degree detection.
Fig. 5, Fig. 6 are the sensitivity characteristic curve graphs of material of the present invention.By 1 products therefrom of embodiment be placed in concentration be 5~
Measured sensitivity characteristic curve graph in the alcohol gas atmosphere of 500ppb, operating temperature are 270 DEG C.Implement as seen from the figure
1 products therefrom of example to the response speed of ethyl alcohol quickly, it is restorative good, and have up to 52 response sensitive the ethyl alcohol of 500ppb
Degree, and the minimum alcohol gas that can detecte 5ppb concentration.
Claims (6)
1. a kind of nano indium oxide gas sensitive for the detection of ppb grades of ethyl alcohol, it is characterised in that: the pattern of the functional material
For laminated structure, the granular size of nanometer sheet is 20~100nm.
2. a kind of preparation method of the nano indium oxide gas sensitive for the detection of ppb grades of ethyl alcohol, it is characterised in that: including following
Processing step:
It is in molar ratio that 1:1~2:3~5 are dissolved in deionized water and are made into metal by indium salts, cetrimonium and sodium hydroxide
Salting liquid, the concentration of indium salts is 0.06~0.08mol/L in the metal salt solution；40~60min is persistently stirred, is allowed to complete
Dissolution is uniformly mixed；Obtained salting liquid is transferred in autoclave again, cooling is sunk after 160 DEG C of 18~20h of reaction
It forms sediment；Finally gained is precipitated through centrifugation, washing, is dried to obtain hydroxide powder, must be received in 350~400 DEG C of 2~3h of calcining
Rice indium oxide functional material.
3. according to the method described in claim 2, it is characterized by: indium salts are five water indium nitrates or inidum chloride.
4. according to the method described in claim 2, it is characterized by: the centrifugation, washing, dry revolving speed when being centrifugal treating
For 4000~8000r/min, carrying out washing treatment is successively to be washed 3~5 times using ethyl alcohol and deionized water, be dried for 60~
Dry 10~20h at 80 DEG C.
5. according to the method described in claim 2, it is characterized by: the calcination process is 3~5 DEG C/min of heating rate, temperature
Degree rises to 350~400 DEG C of 2~3h of holding, is cooled to room temperature naturally in air.
6. a kind of application of the nano indium oxide gas sensitive for the detection of ppb grades of ethyl alcohol, it is characterised in that: nano indium oxide function
Gas sensitive of the energy material as gas sensor, the detection for ppb grades of concentration ethanol gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910705271.XA CN110386620A (en) | 2019-08-01 | 2019-08-01 | Indium oxide gas sensitive and preparation method and application for ppb grades of ethyl alcohol detections |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910705271.XA CN110386620A (en) | 2019-08-01 | 2019-08-01 | Indium oxide gas sensitive and preparation method and application for ppb grades of ethyl alcohol detections |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110386620A true CN110386620A (en) | 2019-10-29 |
Family
ID=68288050
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910705271.XA Pending CN110386620A (en) | 2019-08-01 | 2019-08-01 | Indium oxide gas sensitive and preparation method and application for ppb grades of ethyl alcohol detections |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110386620A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113189148A (en) * | 2021-03-18 | 2021-07-30 | 西安电子科技大学芜湖研究院 | Method for detecting ethanol by indium oxide-based folded microspheres and application |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101109100A (en) * | 2007-07-25 | 2008-01-23 | 中国科学院上海硅酸盐研究所 | Process for producing indium oxide nanocrystalline with controlled shape |
| KR100799577B1 (en) * | 2006-08-31 | 2008-01-30 | 한국전자통신연구원 | Method for forming sensor for detecting gases and biochemical materials, integrated circuit including the sensor, and method for manufacturing the integrated circuit |
| JP2009007235A (en) * | 2007-06-01 | 2009-01-15 | Asahi Kasei Corp | Indium oxide fine particle dispersion |
| CN102234130A (en) * | 2010-05-07 | 2011-11-09 | 广西民族大学 | Simple preparation method of indium oxide nano-cube |
| CN102963922A (en) * | 2012-10-26 | 2013-03-13 | 河南圣玛斯光电科技有限公司 | Hydrothermal synthesis method for indium oxide with cubic crystal structure |
| CN107215890A (en) * | 2017-06-28 | 2017-09-29 | 济南大学 | A kind of preparation method of cubic nanostructures indium oxide gas sensitive |
-
2019
- 2019-08-01 CN CN201910705271.XA patent/CN110386620A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100799577B1 (en) * | 2006-08-31 | 2008-01-30 | 한국전자통신연구원 | Method for forming sensor for detecting gases and biochemical materials, integrated circuit including the sensor, and method for manufacturing the integrated circuit |
| JP2009007235A (en) * | 2007-06-01 | 2009-01-15 | Asahi Kasei Corp | Indium oxide fine particle dispersion |
| CN101109100A (en) * | 2007-07-25 | 2008-01-23 | 中国科学院上海硅酸盐研究所 | Process for producing indium oxide nanocrystalline with controlled shape |
| CN102234130A (en) * | 2010-05-07 | 2011-11-09 | 广西民族大学 | Simple preparation method of indium oxide nano-cube |
| CN102963922A (en) * | 2012-10-26 | 2013-03-13 | 河南圣玛斯光电科技有限公司 | Hydrothermal synthesis method for indium oxide with cubic crystal structure |
| CN107215890A (en) * | 2017-06-28 | 2017-09-29 | 济南大学 | A kind of preparation method of cubic nanostructures indium oxide gas sensitive |
Non-Patent Citations (2)
| Title |
|---|
| YANSONG LI ET AL.: "High-aspect-ratio single-crystalline porous In2O3 nanobelts with enhanced gas sensing properties", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
| 王彬: "不同晶型氧化铟纳米材料的制备及其气敏性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I缉》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113189148A (en) * | 2021-03-18 | 2021-07-30 | 西安电子科技大学芜湖研究院 | Method for detecting ethanol by indium oxide-based folded microspheres and application |
| CN113189148B (en) * | 2021-03-18 | 2024-03-19 | 西安电子科技大学芜湖研究院 | Method for detecting ethanol by using indium oxide-based folded microspheres and application of indium oxide-based folded microspheres |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108663417B (en) | One kind being directed to low concentration of NO2The novel I n of gas2O3/Sb2O3Composite hollow nanotube gas sensitive | |
| Meng et al. | Effects of crystal structure on the activity of MnO 2 nanorods oxidase mimics | |
| CN110194483A (en) | A kind of SnO of multilevel structure2Nano material | |
| CN109916966B (en) | alpha-Fe2O3/TiO2Nanocomposite and H prepared therefrom2S gas sensor | |
| CN105854887B (en) | A kind of cobalt cerium bimetallic oxide nanosphere and preparation method thereof | |
| CN107746069A (en) | The method that hydro-thermal method prepares different-shape ceria | |
| CN109133181A (en) | A kind of rGO-LaFeO3The preparation method of nanocomposite | |
| CN102603016A (en) | Method for preparing nanometer nickel oxide and application of method | |
| Gu et al. | Metal–organic framework derived Au@ ZnO yolk–shell nanostructures and their highly sensitive detection of acetone | |
| CN110386620A (en) | Indium oxide gas sensitive and preparation method and application for ppb grades of ethyl alcohol detections | |
| CN110015698A (en) | A kind of flower-shaped aluminium doped cobaltic-cobaltous oxide and the preparation method and application thereof | |
| CN109115843B (en) | Cu-doped ZnFe2O4Nanoparticles, and preparation method and application thereof | |
| CN107337231B (en) | A kind of preparation method of the hollow hierarchical structure indium oxide of nano particle composition | |
| CN117069165A (en) | Preparation method of Pd modified two-dimensional porous NiO/ZnO gas-sensitive material and method for preparing CO gas sensor by using Pd modified two-dimensional porous NiO/ZnO gas-sensitive material | |
| CN105717178A (en) | Preparation method and application of electrochemical diethylstilbestrol sensor based on titanium-dioxide-based two-dimensional composite nanomaterial | |
| CN109709161A (en) | A kind of tin oxide composite material and preparation method of gold/palldium alloy particle modification and application | |
| CN109019696A (en) | A kind of Au-LaFeO3The preparation method of nanocomposite | |
| CN110243879B (en) | Sulfide ion modified SnO2Low temperature SO2Sensitive material and preparation method thereof | |
| CN107413361A (en) | The method that base metal tungsten carbide photochemical catalyst is prepared using hydro-thermal method | |
| CN108821353A (en) | A kind of RuO2-LaFeO3The preparation method of nanocomposite | |
| CN104198531B (en) | A kind of combined multi-stage structure gas sensitive and preparation method thereof | |
| CN116046726A (en) | Silver nanoparticle modified molybdenum trioxide nanocomposite, preparation method and application thereof | |
| CN115159559A (en) | Oxygen vacancy-containing metal oxide, gas-sensitive composite material, and preparation methods and applications thereof | |
| CN114920280A (en) | MOF-5-based derived ZnO nano-chain material and application thereof | |
| CN114229885A (en) | CdO/SnO2Composite nanocube gas-sensitive material, preparation method and application thereof in hydrogen detection |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191029 |
|
| RJ01 | Rejection of invention patent application after publication |