CN106745194B - The preparation method of ZnO hollow Nano particles - Google Patents
The preparation method of ZnO hollow Nano particles Download PDFInfo
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- CN106745194B CN106745194B CN201611161136.6A CN201611161136A CN106745194B CN 106745194 B CN106745194 B CN 106745194B CN 201611161136 A CN201611161136 A CN 201611161136A CN 106745194 B CN106745194 B CN 106745194B
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003708 ampul Substances 0.000 claims abstract description 22
- 238000001816 cooling Methods 0.000 claims abstract description 22
- 239000010453 quartz Substances 0.000 claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000007864 aqueous solution Substances 0.000 claims abstract description 19
- 238000000889 atomisation Methods 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 241000549556 Nanos Species 0.000 claims abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000001301 oxygen Substances 0.000 claims abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims abstract description 7
- 238000009434 installation Methods 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 150000002431 hydrogen Chemical class 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 239000007789 gas Substances 0.000 abstract description 2
- 238000000151 deposition Methods 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
Classifications
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
-
- B01J35/39—
-
- 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
- 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
-
- 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
- C01P2004/04—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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
-
- 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
Abstract
The invention discloses a kind of preparation method of ZnO hollow Nanos particle, by Zn (CH3COO)2·2H2O is added in deionized water, stirring, is configured to the aqueous solution；The aqueous solution prepared is produced into atomization droplet by atomizer；Atomization droplet is fully burnt by entering after quartz ampoule in hydrogen and oxygen mixed flame, and comburant is deposited to collect in quartz ampoule and collected, and produces ZnO hollow Nano particles.Traditional FSP methods are done to improve, hydrogen is changed to by disposing water cooling plant, and by traditional burning gases methane, hydrogen, which substitutes methane and can avoid collecting in sample, carbon occurs, obtain uniform particle sizes and hollow ZnO nano particle, it is possible to increase the activity of ZnO catalysis materials.
Description
Technical field
The invention belongs to field of environment engineering technology, is related to a kind of preparation method of ZnO hollow Nanos particle.
Background technology
With ZnO and titanium dioxide (TiO2) be representative conductor photocatalysis material so that effectively administer and control water be dirty
Dye and atmosphere pollution are possibly realized.
The factor of influence ZnO photocatalysis performances is a lot, and the main regulation and control including intrinsic defect, surface topography control, are other
Material cladding structure, wherein hollow-core construction are significant for the photocatalysis performance for improving oxide.
And traditional oxide nano particles preparation method is not only difficult to the particle that prepared sizes are evenly distributed, can not accomplish
Hollow-core construction, therefore be difficult the performance for improving catalysis material.
The oxide of even particle size distribution can be obtained by flame atomizing method (flame spray pyrolysis, FSP)
Nano particle, but by many experiments, the particle for finding to finally obtain is also easy to produce reunion, should not be answered in field of environment engineering
With.
The content of the invention
To achieve the above object, the present invention provides a kind of preparation method of ZnO hollow Nanos particle, substantially increases ZnO
The photocatalysis performance of nano particle.
The technical solution adopted in the present invention is a kind of preparation method of ZnO hollow Nanos particle, to enter according to following steps
OK：
Step 1, by Zn (CH3COO)2·2H2O is added in deionized water, stirring, is configured to the aqueous solution；
Step 2, the aqueous solution prepared is produced into atomization droplet by atomizer；
Step 3, it is atomized droplet fully to burn by after quartz ampoule entering in hydrogen and oxygen mixed flame, comburant deposition
Collected to collecting in quartz ampoule, produce ZnO hollow Nano particles.
Further, in the step 3, the conduit wall end installation water cooling plant in quartz ampoule is collected.
Further, in the step 3, the cooling velocity of water cooling is 1.2m/s.
Further, in the step 1, the concentration of the aqueous solution is 0.05~0.5molL-1。
Further, in the step 1, when mixing time is 2~4h, stir speed (S.S.) is 100~500rpm.
Further, in the step 2, atomization rates are 0.05~0.5mL/min.
Further, in the step 3, H2：O2Volume flow ratio be 1~2, ignition temperature is in 2500~3500K.
Further, in the step 3, acquisition time is 2~4h.
Beneficial effects of the present invention：Traditional FSP methods are done to improve, by disposing water cooling plant, and will be traditional
Burning gases methane is changed to hydrogen, and hydrogen, which substitutes methane and can avoid collecting in sample, carbon occurs, obtains uniform particle sizes and sky
The ZnO nano particle of the heart, it is possible to increase the activity of ZnO catalysis materials.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is the XRD spectra of hollow ZnO nano particle made from the embodiment of the present invention.
Fig. 2 a are hollow ZnO nano particle transmission electron microscopy pattern photos made from the embodiment of the present invention, and Fig. 2 b are these
The electronic diffraction pattern photo of hollow ZnO nano particle made from inventive embodiments.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other under the premise of creative work is not made
Embodiment, belong to the scope of protection of the invention.
The preparation method of ZnO hollow Nano particles, is specifically followed the steps below：
Step 1, by Zn (CH3COO)2·2H2O is added in deionized water, is stirred at room temperature, and is configured to the aqueous solution；
Step 2, the aqueous solution prepared is produced into atomization droplet by atomizer；
Step 3, it is atomized droplet fully to burn by after quartz ampoule entering in hydrogen and oxygen mixed flame, comburant deposition
Collected to collecting in quartz ampoule；The pipe wall position installation water cooling plant of the collection quartz ampoule, collect the sample of deposition；
Step 4, by carrying out X-ray diffraction (XRD) test and transmission electron microscope (TEM) analysis, card to the sample of collection
Full pattern product are hollow shape ZnO nano particle.
Wherein, in step 1, the concentration of obtained aqueous solution is 0.05~0.5molL-1。
In step 1, when mixing time is 2~4h, stir speed (S.S.) is 100~500rpm.
In step 2, atomization rates are 0.05~0.5mL/min.Caused atomization droplet size is rear under the speed
The satisfied hollow ZnO nano particle of single-size could be made in continuous burning, Cooling Process.
In step 3, H2：O2Volume flow ratio be 1~2 (SCCM), ignition temperature is adjusted by the ratio of hydrogen and oxygen
Section, scope is in 2500~3500K.
In step 3, acquisition time is 2~4h.
In step 3, the temperature that can bear of selection quartz ampoule is in 1500K, therefore the sample obtained is by can be with after air-flow
Directly collected in tube wall.
In step 3, water cooling plant be arranged on quartz ampoule conduit wall end, cooling velocity 1.2m/s, deposition velocity by
Atomization speed is determined that the sample for not adding the place deposition of cooling water is solid ZnO nano particle.
Embodiment 1
Step 1, by Zn (CH3COO)2·2H2O is added in deionized water and stirred, when mixing time is 2h, stir speed (S.S.)
For 500rpm, the aqueous solution is configured to, the concentration of the aqueous solution is 0.05molL-1；
Step 2, the aqueous solution prepared is produced into atomization droplet, atomization rates 0.05mL/min by atomizer；
Step 3, it is atomized droplet fully to burn by after quartz ampoule entering in hydrogen and oxygen mixed flame, H2：O2Volume
Flow-rate ratio is 1~2, and in 2500K, comburant is deposited to collect in quartz ampoule and collected ignition temperature, collects the tube wall in quartz ampoule
Water cooling plant is installed in end, and the cooling velocity of water cooling is 1.2m/s, acquisition time 2h, produces ZnO hollow Nano particles.
Embodiment 2
Step 1, by Zn (CH3COO)2·2H2O is added in deionized water and stirred, when mixing time is 4h, stir speed (S.S.)
For 100rpm, the aqueous solution is configured to, the concentration of the aqueous solution is 0.5molL-1；
Step 2, the aqueous solution prepared is produced into atomization droplet, atomization rates 0.5mL/min by atomizer；
Step 3, it is atomized droplet fully to burn by after quartz ampoule entering in hydrogen and oxygen mixed flame, H2：O2Volume
Flow-rate ratio is 1~2, and in 3500K, comburant is deposited to collect in quartz ampoule and collected ignition temperature, collects the tube wall in quartz ampoule
Water cooling plant is installed in end, and the cooling velocity of water cooling is 1.2m/s, acquisition time 4h, produces ZnO hollow Nano particles.
Embodiment 3
Step 1, by Zn (CH3COO)2·2H2O is added in deionized water and stirred, when mixing time is 3h, stir speed (S.S.)
For 300rpm, the aqueous solution is configured to, the concentration of the aqueous solution is 0.2molL-1；
Step 2, the aqueous solution prepared is produced into atomization droplet, atomization rates 0.2mL/min by atomizer；
Step 3, it is atomized droplet fully to burn by after quartz ampoule entering in hydrogen and oxygen mixed flame, H2：O2Volume
Flow-rate ratio is 1~2, and in 3000K, comburant is deposited to collect in quartz ampoule and collected ignition temperature, collects the tube wall in quartz ampoule
Water cooling plant is installed in end, and the cooling velocity of water cooling is 1.2m/s, acquisition time 3h, produces ZnO hollow Nano particles.
Hollow ZnO nano preparation method of granules of the present invention, by carrying out tem analysis to it, such as Fig. 2 a, Fig. 2 b institute
Show, it was demonstrated that gained sample is hollow shape ZnO nano particle.Compared with traditional FSP methods, adding after water cooling plant not only can be with
Hollow shape ZnO nano particle is obtained, and the hollow ZnO nano particle photocatalytic activity obtained carries than solid ZnO nano particle
It is high by 30%.Hollow Nano preparation method of granules of the present invention is simple to operate, easy to spread.
Using the method for embodiment 3, the different radial diffraction peaks of obtained product, as can be seen from Figure 1 ZnO, therefrom
ZnO grain size can be calculated.Grain size made from this paper is about 20nm, and different radial direction peaks can be counted in Fig. 1
Calculate, can also intuitively be found out from Fig. 2 a, and the product that can be seen that this paper does not produce the effect of reunion.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the scope of the present invention.It is all
Any modification, equivalent substitution and improvements made within the spirit and principles in the present invention etc., are all contained in protection scope of the present invention
It is interior.
Claims (5)
1. a kind of preparation method of ZnO hollow Nanos particle, it is characterised in that follow the steps below：
Step 1, by Zn (CH3COO)2·2H2O is added in deionized water, stirring, is configured to the aqueous solution；
Step 2, the aqueous solution prepared is produced into atomization droplet by atomizer；
Step 3, it is atomized droplet fully to burn by after quartz ampoule entering in hydrogen and oxygen mixed flame, comburant deposits to receipts
Collect in quartz ampoule and collect, produce ZnO hollow Nano particles；
In the step 3, the conduit wall end installation water cooling plant in quartz ampoule is collected；
In the step 3, the cooling velocity of water cooling is 1.2m/s；
In the step 2, atomization rates are 0.05~0.5mL/min.
2. the preparation method of ZnO hollow Nanos particle according to claim 1, it is characterised in that in the step 1, water
The concentration of solution is 0.05~0.5molL-1。
3. the preparation method of ZnO hollow Nanos particle according to claim 1, it is characterised in that in the step 1, stir
When to mix the time be 2~4h, stir speed (S.S.) is 100~500rpm.
4. the preparation method of ZnO hollow Nanos particle according to claim 1, it is characterised in that in the step 3, H2：
O2Volume flow ratio be 1~2, ignition temperature is in 2500~3500K.
5. the preparation method of ZnO hollow Nanos particle according to claim 1, it is characterised in that in the step 3, receive
The collection time is 2~4h.
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| CN201611161136.6A CN106745194B (en) | 2016-12-15 | 2016-12-15 | The preparation method of ZnO hollow Nano particles |
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| CN201611161136.6A CN106745194B (en) | 2016-12-15 | 2016-12-15 | The preparation method of ZnO hollow Nano particles |
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| CN106745194B true CN106745194B (en) | 2017-12-29 |
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| CN108940259B (en) * | 2018-03-21 | 2020-07-31 | 中国矿业大学 | Hierarchical porous MoO2Photocatalyst microsphere and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1564784A (en) * | 2001-10-05 | 2005-01-12 | 德古萨股份公司 | Aluminum oxide produced by flame hydrolysis and doped with divalent metal oxides and aqueous dispersions thereof |
| CN101219776A (en) * | 2008-01-23 | 2008-07-16 | 上海大学 | Method and device for manufacturing non-glomeration nano-oxide powder body |
-
2016
- 2016-12-15 CN CN201611161136.6A patent/CN106745194B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1564784A (en) * | 2001-10-05 | 2005-01-12 | 德古萨股份公司 | Aluminum oxide produced by flame hydrolysis and doped with divalent metal oxides and aqueous dispersions thereof |
| CN101219776A (en) * | 2008-01-23 | 2008-07-16 | 上海大学 | Method and device for manufacturing non-glomeration nano-oxide powder body |
Non-Patent Citations (3)
| Title |
|---|
| Effect of annealing atmosphere on the photoluminescence of ZnO nanospheres;Yongzhe Zhang et al.,;《Applied Surface Science》;20081211;第255卷;第4801-4805页 * |
| ＺｎＯ纳米颗粒的分散及光致发光特性;李晖等;《陕西科技大学学报》;20130228;第31卷(第1期);第29-32页 * |
| 火焰喷雾法合成ZnO 和MgxZn1 -xO纳米颗粒的光学性能研究;李晖等;《物理学报》;20070630;第56卷(第6期);第3584-3588页 * |
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