CN109319824A - A kind of three-dimensional multistage ZnO/C3N4The preparation method of nanocomposite - Google Patents
A kind of three-dimensional multistage ZnO/C3N4The preparation method of nanocomposite Download PDFInfo
- Publication number
- CN109319824A CN109319824A CN201811291834.7A CN201811291834A CN109319824A CN 109319824 A CN109319824 A CN 109319824A CN 201811291834 A CN201811291834 A CN 201811291834A CN 109319824 A CN109319824 A CN 109319824A
- Authority
- CN
- China
- Prior art keywords
- zno
- nanocomposite
- dimensional
- preparation
- concentration
- 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
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- 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
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention belongs to nanocomposite technical field more particularly to a kind of three-dimensional multistage ZnO/C3N4The preparation method of nanocomposite.The present invention provides a kind of preparation methods of three-dimensional multistage ZnO/C3N4 nanocomposite with acetone and nitrogen oxides hypersensitivity, prepared three-dimensional multistage ZnO/C3N4 nanocomposite can be used as the gas sensor for having hypersensitivity to acetone, including having many advantages, such as selective response to acetone gas and oxides of nitrogen gas, and it is higher to the minimum detection limit of acetone gas and oxides of nitrogen gas.Nanocomposite of the invention is to the gas sensing property of acetone gas not by the interference of ambient humidity；It can be used for clinical breathing gas and photochemical catalyst field.
Description
Technical field
The invention belongs to nanocomposite technical field more particularly to a kind of three-dimensional multistage ZnO/C3N4Nano combined material
The preparation method of material.
Background technique
With the development of science and technology, nanocomposite is more applied in production and living, nano combined material
Expect to realize many traditional technologies in the application of catalyst, structural material and chemical industry chemical field and technique cannot achieve
Effect, meanwhile, the structure and characteristic of nanocomposite itself add its process for producing with tradition is different from
The different manufacturing process of work method.Under normal circumstances, the preparation production of nanocomposite has relatively stringent production
Condition and the limitation of the demand of material and facility, therefore the production capacity of nanocomposite is limited, cannot make it a wide range of well
It is utilized, limits the ability of nano combined mass production, and then limit the ability of nanocomposite production application,
It is unfavorable for the popularization and application of nanocomposite.
Summary of the invention
The present invention analyzes in view of the above technology, provides a kind of three-dimensional multistage with acetone and nitrogen oxides hypersensitivity
The preparation method of ZnO/C3N4 nanocomposite, prepared three-dimensional multistage ZnO/C3N4 nanocomposite can be used as to third
Ketone has the gas sensor of hypersensitivity, including has selective response to acetone gas and oxides of nitrogen gas, and to acetone
The advantages that minimum detection limit of gas and oxides of nitrogen gas is higher.The air-sensitive of nanocomposite of the invention to acetone gas
Property is not by the interference of ambient humidity；It can be used for clinical breathing gas and photochemical catalyst field.
The present invention adopts the following technical scheme:
A kind of three-dimensional multistage ZnO/C3N4The preparation method of nanocomposite, includes the following steps:
Step 1, by the aqueous solution of the aqueous solution of the NaOH of 20 parts by volume and SDS and Zn (NO3) 2+6H2O of 20 parts by volume
The concentration for being mixed to get Zn (NO3) 2 is 0.20mol/L, and the concentration of NaOH is 1.20mol/L, and the concentration of SDS is 0.01mol/L
Mixed aqueous solution, stir 1h, be transferred in ptfe autoclave, be cooled to room temperature, be collected by centrifugation after incubation water heating 15h
Products therefrom is washed with deionized water and dehydrated alcohol, and three-dimensional ZnO nano flower monomer is obtained after vacuum drying；
Melamine is roasted 2h in 550 DEG C of closed atmospheres by step 2, adds ethylene glycol by the super of 1200W/min
Sonication 2h is centrifuged 5min with the speed of 1000r/min, retains upper liquid and obtains C3N4Micron chip；
Step 3, spent glycol make solvent, by the three-dimensional ZnO nano flower monomer and C of preparation3N4The mixing of micron chip carrier, obtains
Concentration to ZnO monomer is 0.008mol/L, C3N4The concentration of carrier is the mixed solution of 0.002mol/L；Ultrasonic agitation is uniform
After be transferred in ptfe autoclave, incubating solvent thermal response 16h is centrifuged after cooling and obtains after being washed with dehydrated alcohol
Three-dimensional multistage ZnO/C3N4Nanocomposite.
To aforementioned three-dimensional multistage ZnO/C3N4The preparation method of nanocomposite, further improvement lies in that, hydro-thermal reaction
Temperature is 90 DEG C, and solvent thermal reaction is 85 DEG C.
To aforementioned three-dimensional multistage ZnO/C3N4The preparation method of nanocomposite, further improvement lies in that, three-dimensional ZnO
Nano flower monomer is 2~4 μm by diameter, and length is accumulated in 1~1.5 μm or so of rodlike construction unit towards different directions.
To aforementioned three-dimensional multistage ZnO/C3N4The preparation method of nanocomposite, further improvement lies in that, C3N4Micron
Piece is 2~8 μm by width, is formed by stacking with a thickness of the micron layer of 20~50nm.
The present invention has the advantages that
1. low-temperature hydrothermal of the present invention/solvent structure three-dimensional multistage ZnO/C3N4 nanocomposite side
Method is easy to operate, lower cost for material, environmentally friendly, repeatable strong, is suitable for industrial mass production, is conducive to its popularization
Using.
2. ZnO/C3N4 nanocomposite prepared by the present invention is accumulated by three-dimensional ZnO nano flower monomer and lamella
Three-dimensional hierarchical structure made of the assembling of C3N4 micron chip carrier.Prepared three-dimensional multistage ZnO/C3N4 nanocomposite is available
In sensor material, photochemical catalyst, catalyst carrier material etc., effect is good, and quality stability is high, before having a wide range of applications
Scape.
3. the preparation method employed in the present invention for preparing ZnO nano flower monomer, ZnO nano flower monomer yield is up to
88.4%；And the preparation method for preparing ZnO/C3N4 nanocomposite used, the yield of ZnO/C3N4 nanocomposite
Up to 71%, it is suitable for batch production..
Specific embodiment
It elaborates below in conjunction with specific embodiment to the invention.
A kind of three-dimensional multistage ZnO/C3N4The preparation method of nanocomposite prepares ZnO/C3N4Nanocomposite
Raw material are Zn (NO3) 2+6H2O, NaOH, SDS, deionized water, melamine, ethyl alcohol and ethylene glycol.
The preparation method of three-dimensional ZnO nano flower monomer uses low-temperature hydrothermal process, by the processing of centrifugation, washing, drying,
The diameter of ZnO nano flower is 2~4 μm, and the rodlike construction unit by many length at 1~1.5 μm or so is accumulated towards different directions
It forms；C3N4Micron chip is fired melamine and obtains, and is 2~8 μm by width, and thickness is only the micron layer superposition of 20~50nm
It forms；Three-dimensional multistage ZnO/C3N4The preparation method of nanocomposite uses low-temperature solvent thermal process, by being centrifuged and with anhydrous
Ethanol washing is for several times；
Its specific three-dimensional multistage ZnO/C3N4The preparation method of nanocomposite includes the following steps:
Step 1, by the aqueous solution of the aqueous solution of the NaOH of 20 parts by volume and SDS and Zn (NO3) 2+6H2O of 20 parts by volume
The concentration for being mixed to get Zn (NO3) 2 is 0.20mol/L, and the concentration of NaOH is 1.20mol/L, and the concentration of SDS is 0.01mol/L
Mixed aqueous solution, stir 1h, be transferred in ptfe autoclave, be cooled to room temperature after incubation water heating 15h, hydro-thermal reaction
Temperature is 90 DEG C, and products therefrom is collected by centrifugation, is washed with deionized water and dehydrated alcohol, three-dimensional ZnO is obtained after vacuum drying and is received
Popped rice monomer；Three-dimensional ZnO nano flower monomer is 2~4 μm by diameter, and length is in 1~1.5 μm or so of rodlike construction unit towards not
It is equidirectional to accumulate.
Melamine is roasted 2h in 550 DEG C of closed atmospheres by step 2, adds ethylene glycol by the super of 1200W/min
Sonication 2h is centrifuged 5min with the speed of 1000r/min, retains upper liquid and obtains C3N4Micron chip；C3N4Micron chip is by width
It 2~8 μm, is formed by stacking with a thickness of the micron layer of 20~50nm.
Step 3, spent glycol make solvent, by the three-dimensional ZnO nano flower monomer and C of preparation3N4The mixing of micron chip carrier, obtains
Concentration to ZnO monomer is 0.008mol/L, C3N4The concentration of carrier is the mixed solution of 0.002mol/L；Ultrasonic agitation is uniform
After be transferred in ptfe autoclave, incubating solvent thermal response 16h, solvent thermal reaction is 85 DEG C, is centrifuged and is used in combination after cooling
Three-dimensional multistage ZnO/C is obtained after dehydrated alcohol washing3N4Nanocomposite.
Finally it should be noted that above embodiments are only to illustrate the technical solution of the invention, rather than to this hair
It is bright create protection scope limitation, although being explained in detail referring to preferred embodiment to the invention, this field it is general
Lead to it will be appreciated by the skilled person that can be modified or replaced equivalently to the technical solution of the invention, without departing from this
The spirit and scope of innovation and creation technical solution.
Claims (4)
1. a kind of three-dimensional multistage ZnO/C3N4The preparation method of nanocomposite, which comprises the steps of:
Step 1 mixes the aqueous solution of the NaOH of 20 parts by volume and SDS with the aqueous solution of Zn (NO3) 2+6H2O of 20 parts by volume
The concentration for obtaining Zn (NO3) 2 is 0.20mol/L, and the concentration of NaOH is 1.20mol/L, and the concentration of SDS is the mixed of 0.01mol/L
Heshui solution stirs 1h, is transferred in ptfe autoclave, is cooled to room temperature after incubation water heating 15h, and gained is collected by centrifugation
Product is washed with deionized water and dehydrated alcohol, and three-dimensional ZnO nano flower monomer is obtained after vacuum drying；
Melamine is roasted 2h in 550 DEG C of closed atmospheres by step 2, is added ethylene glycol and is passed through at the ultrasound of 1200W/min
2h is managed, 5min is centrifuged with the speed of 1000r/min, retains upper liquid and obtains C3N4Micron chip；
Step 3, spent glycol make solvent, by the three-dimensional ZnO nano flower monomer and C of preparation3N4The mixing of micron chip carrier, obtains ZnO
The concentration of monomer is 0.008mol/L, C3N4The concentration of carrier is the mixed solution of 0.002mol/L；Ultrasonic agitation uniformly rear transfer
Into ptfe autoclave, incubating solvent thermal response 16h, is centrifuged after cooling and to obtain three-dimensional after being washed with dehydrated alcohol more
Grade ZnO/C3N4Nanocomposite.
2. a kind of three-dimensional multistage ZnO/C according to claim 13N4The preparation method of nanocomposite, which is characterized in that
Hydrothermal temperature is 90 DEG C, and solvent thermal reaction is 85 DEG C.
3. a kind of three-dimensional multistage ZnO/C according to claim 13N4The preparation method of nanocomposite, which is characterized in that
The three-dimensional ZnO nano flower monomer is 2~4 μm by diameter, and length is in 1~1.5 μm or so of rodlike construction unit towards not Tongfang
To accumulating.
4. a kind of three-dimensional multistage ZnO/C according to claim 13N4The preparation method of nanocomposite, which is characterized in that
The C3N4Micron chip is 2~8 μm by width, is formed by stacking with a thickness of the micron layer of 20~50nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811291834.7A CN109319824A (en) | 2018-10-31 | 2018-10-31 | A kind of three-dimensional multistage ZnO/C3N4The preparation method of nanocomposite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811291834.7A CN109319824A (en) | 2018-10-31 | 2018-10-31 | A kind of three-dimensional multistage ZnO/C3N4The preparation method of nanocomposite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109319824A true CN109319824A (en) | 2019-02-12 |
Family
ID=65259948
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811291834.7A Pending CN109319824A (en) | 2018-10-31 | 2018-10-31 | A kind of three-dimensional multistage ZnO/C3N4The preparation method of nanocomposite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109319824A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110044971A (en) * | 2019-04-16 | 2019-07-23 | 蚌埠学院 | A kind of gas sensitive, preparation method and its application in gas sensor |
| CN113755031A (en) * | 2021-10-22 | 2021-12-07 | 安徽锦华氧化锌有限公司 | Dispersing and activating treatment method for zinc oxide |
| CN114560492A (en) * | 2022-02-16 | 2022-05-31 | 西北大学 | N-graphene/ZnO composite gas-sensitive material, preparation method and application |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104084228A (en) * | 2014-06-25 | 2014-10-08 | 华南理工大学 | Oxygen-doped carbon nitride/zinc oxide photo-catalyst as well as preparation method and application thereof |
| CN104437649A (en) * | 2013-09-24 | 2015-03-25 | 中国地质大学（北京） | ZnO/mesoporous C3N4 composite photocatalyst and preparation method thereof |
| CN108212191A (en) * | 2018-01-15 | 2018-06-29 | 吉林师范大学 | A kind of preparation method of zinc oxide nitridation carbon quantum dot composite construction visible light catalyst |
| CN108246241A (en) * | 2018-03-15 | 2018-07-06 | 长沙理工大学 | One kind is by helical form g-C3N4The sea urchin type superstructure material of/ZnO composite nanorods assembling |
-
2018
- 2018-10-31 CN CN201811291834.7A patent/CN109319824A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437649A (en) * | 2013-09-24 | 2015-03-25 | 中国地质大学（北京） | ZnO/mesoporous C3N4 composite photocatalyst and preparation method thereof |
| CN104084228A (en) * | 2014-06-25 | 2014-10-08 | 华南理工大学 | Oxygen-doped carbon nitride/zinc oxide photo-catalyst as well as preparation method and application thereof |
| CN108212191A (en) * | 2018-01-15 | 2018-06-29 | 吉林师范大学 | A kind of preparation method of zinc oxide nitridation carbon quantum dot composite construction visible light catalyst |
| CN108246241A (en) * | 2018-03-15 | 2018-07-06 | 长沙理工大学 | One kind is by helical form g-C3N4The sea urchin type superstructure material of/ZnO composite nanorods assembling |
Non-Patent Citations (3)
| Title |
|---|
| NING ZHANG等: "In situ hydrothermal growth of ZnO/g-C3N4 nanoflowers coated solid-phase microextraction fibers coupled with GC-MS for determination of pesticides residues", 《ANALYTICA CHIMICA ACTA》 * |
| S. L. BAI等: "Synthesis of 1D ZnO Crystals and Sensing Properties for NO2 Gas", 《IEEE SENSORS JOURNAL》 * |
| SURYA PRASAD ADHIKARI等: "Deposition of ZnO flowers on the surface of g-C3N4 sheets via hydrothermal process", 《CERAMICS INTERNATIONAL》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110044971A (en) * | 2019-04-16 | 2019-07-23 | 蚌埠学院 | A kind of gas sensitive, preparation method and its application in gas sensor |
| CN110044971B (en) * | 2019-04-16 | 2021-11-23 | 蚌埠学院 | Gas-sensitive material, preparation method and application thereof in gas-sensitive sensor |
| CN113755031A (en) * | 2021-10-22 | 2021-12-07 | 安徽锦华氧化锌有限公司 | Dispersing and activating treatment method for zinc oxide |
| CN114560492A (en) * | 2022-02-16 | 2022-05-31 | 西北大学 | N-graphene/ZnO composite gas-sensitive material, preparation method and application |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109319824A (en) | A kind of three-dimensional multistage ZnO/C3N4The preparation method of nanocomposite | |
| CN105732860B (en) | The expandable polystyrene bead and preparation method of inflatable few layer graphene | |
| CN101318646B (en) | Method for preparing TiO2 coated carbon nano-tube composite material | |
| CN105271371B (en) | A kind of flower-shaped indium oxide micron bar material and its preparation method and application | |
| CN103101967A (en) | Preparation method three-dimensional multistage SnO2 nanoflowers | |
| CN106745285B (en) | A kind of α-MnO2The preparation method of nano wire | |
| CN104891556B (en) | Zinc hydroxystannate in double-layer hollow cubic structure and preparation method thereof | |
| CN104817106B (en) | TiO2The solvent process for thermosynthesizing of hollow-core construction sub-micron ball | |
| CN105238349B (en) | A kind of Fe3O4ZnO nano composite and preparation method thereof | |
| CN106866992B (en) | A kind of preparation method of the titania modified polyacrylate dispersion of hollow spheres | |
| CN111019152A (en) | Method for ultrasonic-assisted synthesis of zirconium-based metal organic framework material and product thereof | |
| CN106969860A (en) | Intelligent Magnetic driving selfreparing flexible pressure-sensitive sensor and preparation method thereof | |
| CN106186048B (en) | A kind of preparation method of the hierarchy indium oxide microballoon of cube composition | |
| CN104877277B (en) | Method for preparing bismuth tungstate/ polyvinylidene fluoride composite material | |
| CN105565375A (en) | Preparing method for nanoscale porous titanium dioxide hollow spheres | |
| CN104556217B (en) | A kind of method preparing divalent metal titanate microballoon | |
| CN103482682B (en) | Preparation method of HEPES (hydroxyethylpiperazine ethane sulfonic acid) molecule guided porous zinc oxide microspheres | |
| CN105800693B (en) | A kind of preparation method of α FeOOH three-dimensional multistage microballoons | |
| CN104229878A (en) | Preparation method of rutile crystal-form titanium dioxide nanorod | |
| CN108776156A (en) | One-dimensional α-Fe2O3The preparation method of nanometer rods and be based on α-Fe2O3The acetone sensor of nanometer rods | |
| CN105271374A (en) | Preparation method of stannic oxide microspheres of oriented connection microstructure | |
| CN106927501A (en) | A kind of hollow core shell structure TiO for gas sensing2Mesoporous microsphere and its controllable method for preparing | |
| CN104671291B (en) | A kind of velvet flowers shape Fe of micro nano structure3O4And preparation method thereof | |
| CN105271421A (en) | Preparation method of tungsten-based nanosphere particle powder | |
| CN101723437A (en) | Method for preparing porous laminated zinc oxide sphere |
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: 20190212 |
|
| RJ01 | Rejection of invention patent application after publication |