CN104445367A - Preparation method of nanoflower-shaped zinc oxide - Google Patents
Preparation method of nanoflower-shaped zinc oxide Download PDFInfo
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- CN104445367A CN104445367A CN201410640910.6A CN201410640910A CN104445367A CN 104445367 A CN104445367 A CN 104445367A CN 201410640910 A CN201410640910 A CN 201410640910A CN 104445367 A CN104445367 A CN 104445367A
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention discloses a preparation method of nanoflower-shaped zinc oxide. The preparation method specifically comprises the following steps: preparing a zinc salt aqueous solution; dropwise adding an alkaline solution into the zinc salt aqueous solution till the zinc salt aqueous solution is strongly alkaline to form a reaction liquid; putting the reaction liquid into a liner of a hydrothermal reaction kettle; screwing the hydrothermal reaction kettle and putting the kettle into an oven to react; taking out the hydrothermal reaction kettle and cooling at room temperature, centrifugalizing the reaction liquid to obtain a white precipitate and respectively cleaning the white precipitate alternately by using absolute ethyl alcohol and deionized water; and putting the cleaned white precipitate into the oven to be dried at 60-100 DEG C to obtain ZnO powder in a nanoflower-shaped structure, wherein the pedal is a nanosheet which is about 30nm thick. The raw materials are easily available, and the preparation method has the characteristics of simple equipment process, high yield, low preparation cost and the like and is suitable for industrial production on a large scale.
Description
Technical field
The present invention relates to nano material technology, particularly relate to a kind of preparation method of nanoscale flower-like zinc oxide.
Background technology
Zinc oxide is a kind of important semiconductor material with wide forbidden band, because its special structure makes this material show many specific functions in catalysis, optics, magnetics, mechanics etc., be widely used in the optoelectronic areas such as photodiode, gas sensor, ultraviolet detector.Nano zine oxide is because its size is between cluster and Macroscopic particulates, there is volume (small size) effect of nano material, surface effects and macro quanta tunnel effect, in optical, electrical, air-sensitive, antibiotic and sterilizing, ultraviolet screener etc., possess the specific function not available for common zinc oxide product.In recent years about the preparation of nano zinc oxide material, performance and applied research are paid close attention to widely.Due to the structure of material and the performance of pattern and material closely related, the preparation of the morphology controllable of ZnO nano material remains a focus of ZnO material research field.The method of current making ZnO nano material has a lot, such as metal organic chemical vapor deposition, hydrothermal method, sol-gel method, electrodip process etc.Wherein hydrothermal method has simply controlled advantage and receives much concern, and therefore control water reaction conditions, the ZnO nano-structure powder preparing good crystalline phase and special appearance has important practical significance.In existing Hydrothermal Synthesis ZnO nano flower-like structure, in precursor solution, usually add auxiliary reagent to control pattern, or in building-up process, obtained the ZnO material of nano flower-like by other auxiliary treatment means.Above-mentioned making method complex operation, controllability is low, cost is higher and easily produce end product and pollute; The nanoscale flower-like zinc oxide pattern integrity degree made is poor, granularity is uneven, purity is lower, hinders the large-scale application of flower-like nanometer zinc oxide.
Summary of the invention
The object of the invention is to the deficiency overcoming prior art, a kind of hydrothermal preparing process of nanoscale flower-like zinc oxide is provided.The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of nanoscale flower-like zinc oxide, comprises the following steps:
The zinc salt solution of A, preparation 0.15-0.4mol/L, wherein zinc salt is selected from zinc sulfate, Zinc diacetate dihydrate, zinc chloride or zinc nitrate hexahydrate;
B, be added drop-wise to until zinc salt solution is strong basicity in zinc salt solution by alkaline solution, forming reactions liquid, wherein alkaline solution is potassium hydroxide or sodium hydroxide, and the pH value range of reaction solution is 11-12;
C, above-mentioned reaction solution is placed in hydrothermal reaction kettle liner; Screw hydrothermal reaction kettle, be placed in baking oven in 120-200 DEG C of reaction 2-5h;
D, taking-up hydrothermal reaction kettle also at room temperature cool, and reaction solution is centrifugal obtains white depositions, by white depositions respectively with dehydrated alcohol and deionized water alternately cleaning;
E, the white depositions after cleaning is placed in baking oven 60-100 DEG C of oven dry, the ZnO powder of acquisition nano flower-like structure.
Preferably, the flower-like structure that described nano flower-like ZnO is made up of the petal design of nanometer sheet unit, wherein the thickness of petal design is 20nm-40nm.
Preferably, the thickness of the petal design of described nano flower-like ZnO is 30nm.
Preferably, the particle size range of described nano flower-like ZnO is 1-2um.
Preferably, the liner of described hydrothermal reaction kettle is tetrafluoroethylene.
Preferably, in step C, the temperature rise rate of hydro-thermal reaction is 10-30 DEG C/min.
The zinc oxide nano-powder that this preparation method obtains is that pure white, epigranular, degree of crystallinity are high, shows that its crystalline structure is consistent with the crystalline structure of standard ZnO (JCPDS (JCPDS) card number: 36-1451) through XRD (X-ray diffraction) test; By field emission microscopy observation, this powder is nano flower-like structure, and petal thickness is the nanometer sheet of about 20-40nm.This preparation method has that abundant raw materials is easy to get, the easy feature such as fast of reaction scheme, and be applicable to large-scale industrial production, tool has been widely used in the industry.
Below in conjunction with drawings and Examples, the present invention is described in further detail; But the preparation method of a kind of nanoscale flower-like zinc oxide of the present invention is not limited to embodiment.
Accompanying drawing explanation
Fig. 1 is the nanoscale flower-like zinc oxide powder x-ray diffraction pattern of one embodiment of the invention;
Fig. 2 is the nanoscale flower-like zinc oxide powder electron scanning micrograph of one embodiment of the invention;
Fig. 3 is the nanoscale flower-like zinc oxide powder of one embodiment of the invention and commercial Zinc oxide powder comparing acetone air-sensitive performance.
Embodiment
Embodiment 1
Get 2.7055g Zn (NO
3)
26H
2o adds 25ml deionized water dissolving, is mixed with the zinc salt solution of 0.37mol/L.Slow dropping potassium hydroxide solution is in zinc salt solution, until the pH value of zinc salt solution is 11, and forming reactions liquid.Reaction solution is placed in hydrothermal reaction kettle polytetrafluoroethyllining lining, screws hydrothermal reaction kettle, be placed in baking oven.Baking oven with the ramp to 200 DEG C of 10 DEG C/min, take out hydrothermal reaction kettle after isothermal reaction 3h and with room temperature under cool.Obtain white depositions after reaction solution is centrifugal, by white depositions dehydrated alcohol and deionized water alternately cleaning, and be placed in 80 DEG C of oven dry in baking oven, obtain the ZnO powder of nano flower-like structure.
As shown in Figure 1, carry out XRD (X-ray diffraction) test to the powder prepared, XRD figure stave its crystalline structure bright is consistent with the crystalline structure of standard ZnO (JCPDS (JCPDS) card number: 36-1451).As shown in Fig. 2 electron scanning micrograph, the flower-like structure that its microcosmic crystalline structure of the powder prepared is made up of the petal design of nanometer sheet unit, wherein the thickness of nanometer sheet petal is about 30nm, and the particle diameter of flower-like structure is 1-2um.
Reaction mechanism of the present invention is:
Zn
2++2OH
-→Zn(OH)
2↓ (1)
Zn(OH)
2+2OH
-→Zn(OH)
4 2-(2)
Zn(OH)
4 2-→ZnO+2H
2O+2OH
-(3)
In strong alkali solution, mainly there is Zn (OH)
4 2-, as Zn (OH)
4 2-a lot of at the ZnO nucleus of aqueous phase formation time dense, nucleus can along all directions ramp, and the crystal face perpendicular to c-axis direction becomes advantage crystal face, ramp slabbing.Nucleus grows towards all directions, causes product with certain crystal face of thin slice for core, constantly grows along all directions, finally forms random flower-like structure interlaced with each other.In the environment of hydrothermal reaction kettle high pressure, the crystal face speed of growth in c-axis direction reduces relatively, is so more conducive to the nanometer sheet forming thinner thickness.
In the present embodiment, the powder purity prepared is high, uniform particle sizes, and flower-like structure is complete, and petal is thin, has a wide range of applications.Such as, zinc oxide is as gas sensitive, and when making gas sensor, the flower-like structure of microcosmic makes its contact area with gas to be measured greatly, and petal design is enough thin, and highly sensitive, air-sensitive performance is more good.See Fig. 3, in the detection for acetone gas concentration, compared with commercially available common zinc oxide powder, its air-sensitive performance of nanoscale flower-like zinc oxide powder of the present invention increases significantly.
Embodiment 2
Get solid sulphuric acid zinc and add deionized water dissolving, be mixed with the zinc salt solution of 0.15mol/L.Slow dropping sodium hydroxide solution is in zinc salt solution, until the pH value of zinc salt solution is 12, and forming reactions liquid.Reaction solution is placed in hydrothermal reaction kettle polytetrafluoroethyllining lining, screws hydrothermal reaction kettle, be placed in baking oven.Baking oven with the ramp to 120 DEG C of 15 DEG C/min, take out hydrothermal reaction kettle after isothermal reaction 5h and with room temperature under cool.Obtain white depositions after reaction solution is centrifugal, by white depositions dehydrated alcohol and deionized water alternately cleaning, and be placed in 60 DEG C of oven dry in baking oven, obtain the ZnO powder of nano flower-like structure.The flower-like structure that the powder prepared is made up of the petal design of nanometer sheet unit, wherein the thickness of nanometer sheet petal is 20-40nm, and the particle diameter of flower-like structure is 1-2um.
Embodiment 3
Get solid zinc acetate and add deionized water dissolving, be mixed with the zinc salt solution of 0.3mol/L.Slow dropping potassium hydroxide solution is in zinc salt solution, until the pH value of zinc salt solution is 11, and forming reactions liquid.Reaction solution is placed in hydrothermal reaction kettle polytetrafluoroethyllining lining, screws hydrothermal reaction kettle, be placed in baking oven.Baking oven with the ramp to 140 DEG C of 20 DEG C/min, take out hydrothermal reaction kettle after isothermal reaction 4h and with room temperature under cool.Obtain white depositions after reaction solution is centrifugal, by white depositions dehydrated alcohol and deionized water alternately cleaning, and be placed in 70 DEG C of oven dry in baking oven, obtain the ZnO powder of nano flower-like structure.The flower-like structure that the powder prepared is made up of the petal design of nanometer sheet unit, wherein the thickness of nanometer sheet petal is 20-40nm, and the particle diameter of flower-like structure is 1-2um.
Embodiment 4
Get zinc chloride and add deionized water dissolving, be mixed with the zinc salt solution of 0.4mol/L.Slow dropping potassium hydroxide solution is in zinc salt solution, until the pH value of zinc salt solution is 11, and forming reactions liquid.Reaction solution is placed in hydrothermal reaction kettle polytetrafluoroethyllining lining, screws hydrothermal reaction kettle, be placed in baking oven.Baking oven with the ramp to 180 DEG C of 30 DEG C/min, take out hydrothermal reaction kettle after isothermal reaction 2h and with room temperature under cool.Obtain white depositions after reaction solution is centrifugal, by white depositions dehydrated alcohol and deionized water alternately cleaning, and be placed in 100 DEG C of oven dry in baking oven, obtain the ZnO powder of nano flower-like structure.The flower-like structure that the powder prepared is made up of the petal design of nanometer sheet unit, wherein the thickness of nanometer sheet petal is 20-40nm, and the particle diameter of flower-like structure is 1-2um.
Embodiment 5
Get Zn (NO
3)
26H
2o adds deionized water dissolving, is mixed with the zinc salt solution of 0.18mol/L.Slow dropping sodium hydroxide solution is in zinc salt solution, until the pH value of zinc salt solution is 12, and forming reactions liquid.Reaction solution is placed in hydrothermal reaction kettle polytetrafluoroethyllining lining, screws hydrothermal reaction kettle, be placed in baking oven.Baking oven with the ramp to 160 DEG C of 30 DEG C/min, take out hydrothermal reaction kettle after isothermal reaction 5h and with room temperature under cool.Obtain white depositions after reaction solution is centrifugal, by white depositions dehydrated alcohol and deionized water alternately cleaning, and be placed in 90 DEG C of oven dry in baking oven, obtain the ZnO powder of nano flower-like structure.The flower-like structure that the powder prepared is made up of the petal design of nanometer sheet unit, wherein the thickness of nanometer sheet petal is 20-40nm, and the particle diameter of flower-like structure is 1-2um.
Above-described embodiment is only used for further illustrating the preparation method of a kind of nanoscale flower-like zinc oxide structure of the present invention; but the present invention is not limited to embodiment; every above embodiment is done according to technical spirit of the present invention any simple modification, equivalent variations and modification, all fall in the protection domain of technical solution of the present invention.
Claims (6)
1. a preparation method for nanoscale flower-like zinc oxide, is characterized in that comprising the following steps:
The zinc salt solution of A, preparation 0.15-0.4mol/L, wherein zinc salt is selected from zinc sulfate, Zinc diacetate dihydrate, zinc chloride or zinc nitrate hexahydrate;
B, be added drop-wise to until zinc salt solution is strong basicity in zinc salt solution by alkaline solution, forming reactions liquid, wherein alkaline solution is potassium hydroxide or sodium hydroxide, and the pH value range of reaction solution is 11-12;
C, above-mentioned reaction solution is placed in hydrothermal reaction kettle liner; Screw hydrothermal reaction kettle, be placed in baking oven in 120-200 DEG C of reaction 2-5h;
D, taking-up hydrothermal reaction kettle also at room temperature cool, and reaction solution is centrifugal obtains white depositions, by white depositions respectively with dehydrated alcohol and deionized water alternately cleaning;
E, the white depositions after cleaning is placed in baking oven 60-100 DEG C of oven dry, the ZnO powder of acquisition nano flower-like structure.
2. the preparation method of nanoscale flower-like zinc oxide according to claim 1, is characterized in that: the flower-like structure that described nano flower-like ZnO is made up of the petal design of nanometer sheet unit, and wherein the thickness of petal design is 20nm-40nm.
3. the preparation method of nanoscale flower-like zinc oxide according to claim 2, is characterized in that: the thickness of the petal design of described nano flower-like ZnO is 30nm.
4. the preparation method of nanoscale flower-like zinc oxide according to claim 2, is characterized in that: the particle size range of described nano flower-like ZnO is 1-2um.
5. the preparation method of nanoscale flower-like zinc oxide according to claim 1, is characterized in that: the liner of described hydrothermal reaction kettle is tetrafluoroethylene.
6. the preparation method of nanoscale flower-like zinc oxide according to claim 1, is characterized in that: in step C, and the temperature rise rate of hydro-thermal reaction is 10-30 DEG C/min.
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104843768A (en) * | 2015-05-26 | 2015-08-19 | 西安工程大学 | Preparation method for three-dimensional multilayer nanometer zinc oxide |
| CN105215347A (en) * | 2015-09-07 | 2016-01-06 | 济南大学 | A kind of zinc oxide and gold nano grain composite and preparation method thereof |
| CN105540640A (en) * | 2016-01-26 | 2016-05-04 | 东北林业大学 | Preparation method of flower-shaped nanometer zinc oxide |
| CN106186044A (en) * | 2016-07-26 | 2016-12-07 | 陕西科技大学 | A kind of preparation method of flower shape zinc oxide nanometer sheet cluster |
| CN106277027A (en) * | 2016-07-26 | 2017-01-04 | 陕西科技大学 | A kind of preparation method of flower shape zinc oxide nanometer rods cluster |
| CN106966424A (en) * | 2017-05-26 | 2017-07-21 | 贵州大学 | Nano zine oxide and preparation method thereof |
| CN107235506A (en) * | 2017-07-10 | 2017-10-10 | 安徽锦华氧化锌有限公司 | A kind of preparation method of nano zine oxide heterojunction structure |
| CN107737942A (en) * | 2017-10-23 | 2018-02-27 | 南京工程学院 | A kind of Zero-valent Iron/flower shape zinc oxide nano composite material and preparation method thereof |
| CN108273490A (en) * | 2018-04-02 | 2018-07-13 | 哈尔滨理工大学 | A kind of zinc oxide/metatitanic acid yttrium lead and preparation method |
| CN108682872A (en) * | 2018-05-22 | 2018-10-19 | 江苏理工学院 | A kind of preparation method of the nitrogen co-doped grading-hole carbon nanosheet oxygen reduction catalyst of iron cobalt |
| CN108677263A (en) * | 2018-04-11 | 2018-10-19 | 巢湖市瀚海渔具有限公司 | A kind of fishing net with good knotting strength |
| CN109294477A (en) * | 2018-10-30 | 2019-02-01 | 龚娟 | A kind of preparation method of building adhesive |
| CN110124654A (en) * | 2019-05-22 | 2019-08-16 | 天津大学 | A kind of nanoscale flower-like zinc oxide photochemical catalyst and its preparation method and application |
| CN110526228A (en) * | 2019-09-12 | 2019-12-03 | 北京工业大学 | The preparation method of one type petal-shaped carbon nanosheet |
| CN110813272A (en) * | 2019-11-08 | 2020-02-21 | 昆明理工大学 | Preparation method of flower-shaped nano ZnO catalyst |
| CN112915991A (en) * | 2021-01-19 | 2021-06-08 | 西南交通大学 | Preparation method of lamellar aggregated flower-shaped zinc oxide photocatalyst |
| CN113769481A (en) * | 2021-09-28 | 2021-12-10 | 武汉纺织大学 | Organic-inorganic hybrid air filtration protective material with multilevel structure |
| US11325839B2 (en) | 2018-01-11 | 2022-05-10 | Imam Abdulrahman Bin Faisal University | Zinc oxide particle preparation and methods of use |
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| CN104843768A (en) * | 2015-05-26 | 2015-08-19 | 西安工程大学 | Preparation method for three-dimensional multilayer nanometer zinc oxide |
| CN105215347A (en) * | 2015-09-07 | 2016-01-06 | 济南大学 | A kind of zinc oxide and gold nano grain composite and preparation method thereof |
| CN105215347B (en) * | 2015-09-07 | 2017-03-29 | 济南大学 | A kind of Zinc Oxide and gold nano grain composite and preparation method thereof |
| CN105540640A (en) * | 2016-01-26 | 2016-05-04 | 东北林业大学 | Preparation method of flower-shaped nanometer zinc oxide |
| CN105540640B (en) * | 2016-01-26 | 2017-04-26 | 东北林业大学 | Preparation method of flower-shaped nanometer zinc oxide |
| CN106186044A (en) * | 2016-07-26 | 2016-12-07 | 陕西科技大学 | A kind of preparation method of flower shape zinc oxide nanometer sheet cluster |
| CN106277027A (en) * | 2016-07-26 | 2017-01-04 | 陕西科技大学 | A kind of preparation method of flower shape zinc oxide nanometer rods cluster |
| CN106966424A (en) * | 2017-05-26 | 2017-07-21 | 贵州大学 | Nano zine oxide and preparation method thereof |
| CN107235506A (en) * | 2017-07-10 | 2017-10-10 | 安徽锦华氧化锌有限公司 | A kind of preparation method of nano zine oxide heterojunction structure |
| CN107737942A (en) * | 2017-10-23 | 2018-02-27 | 南京工程学院 | A kind of Zero-valent Iron/flower shape zinc oxide nano composite material and preparation method thereof |
| US11325839B2 (en) | 2018-01-11 | 2022-05-10 | Imam Abdulrahman Bin Faisal University | Zinc oxide particle preparation and methods of use |
| CN108273490A (en) * | 2018-04-02 | 2018-07-13 | 哈尔滨理工大学 | A kind of zinc oxide/metatitanic acid yttrium lead and preparation method |
| CN108677263A (en) * | 2018-04-11 | 2018-10-19 | 巢湖市瀚海渔具有限公司 | A kind of fishing net with good knotting strength |
| CN108682872A (en) * | 2018-05-22 | 2018-10-19 | 江苏理工学院 | A kind of preparation method of the nitrogen co-doped grading-hole carbon nanosheet oxygen reduction catalyst of iron cobalt |
| CN109294477A (en) * | 2018-10-30 | 2019-02-01 | 龚娟 | A kind of preparation method of building adhesive |
| CN110124654A (en) * | 2019-05-22 | 2019-08-16 | 天津大学 | A kind of nanoscale flower-like zinc oxide photochemical catalyst and its preparation method and application |
| CN110526228A (en) * | 2019-09-12 | 2019-12-03 | 北京工业大学 | The preparation method of one type petal-shaped carbon nanosheet |
| CN110526228B (en) * | 2019-09-12 | 2021-03-30 | 北京工业大学 | Preparation method of petal-like carbon nanosheets |
| CN110813272A (en) * | 2019-11-08 | 2020-02-21 | 昆明理工大学 | Preparation method of flower-shaped nano ZnO catalyst |
| CN112915991A (en) * | 2021-01-19 | 2021-06-08 | 西南交通大学 | Preparation method of lamellar aggregated flower-shaped zinc oxide photocatalyst |
| CN113769481A (en) * | 2021-09-28 | 2021-12-10 | 武汉纺织大学 | Organic-inorganic hybrid air filtration protective material with multilevel structure |
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