CN104528807A - Preparation method for multibasic oxide nanometer material - Google Patents
Preparation method for multibasic oxide nanometer material Download PDFInfo
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- CN104528807A CN104528807A CN201510002382.6A CN201510002382A CN104528807A CN 104528807 A CN104528807 A CN 104528807A CN 201510002382 A CN201510002382 A CN 201510002382A CN 104528807 A CN104528807 A CN 104528807A
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Abstract
The invention discloses a preparation method for a multibasic oxide nanometer material. The general formula of the nanometer material is AxByOz, wherein A and B are any two of Zn or Ge or Fe or Mn or Ni or Co, the equation that xa+by=2z is met, and a and b are valences of the metallic element A and the metallic element B. The preparation method for the multibasic oxide nanometer material comprises the specific steps that a, two metal target materials are soaked with deionized water, a Nd:YAG pulse laser is used for conducting laser ablation for 5 min to 50 min, and the metal target materials are made to form two colloidal solutions, wherein the metal target materials are any two of Zn or Ge or Fe or Mn or Ni or Co; b, the two obtained colloidal solutions are mixed evenly for 5 min to 10 min to be moved into a high pressure hydrothermal reaction kettle, a reaction is carried out at the temperature ranging from 80 DEG C to 180 DEG C for 6 h, and crystals obtained through the reaction are the multibasic oxide nanometer material. The preparation method is simple in operation steps, no any additional chemical reagent needs to be added in the reaction process, and the preparation method is environmentally friendly.
Description
Technical field
The present invention relates to field of nanometer material technology, particularly a kind of multivariant oxide nano material and preparation method thereof.
Background technology
Multivariant oxide nano material has photoelectricity, electrochemical activity, ferroelectric, the unique property such as multiferroic, nonlinear optics, and at photodetector, Photocatalyzed Hydrogen Production, lithium ion battery, the aspects such as ultracapacitor obtain applying more and more widely, as Zn
2geO
4nano wire, namely has chemistry and thermodynamic stability, and energy gap is larger, and wavelength selectivity is stronger, and deep UV (ultraviolet light) electric explorer has more superior performance.
The conventional method preparing binary oxide has high temperature solid state reaction synthesis method, chemical coprecipitation area method, sol-gel method at present, relative to preparation, these traditional methods all also exist inevitable defect: multicomponent oxide composition granule prepared by high temperature solid state reaction synthesis method is larger, purity is low, high temperature easily causes chemical constitution to be more difficult to control, and can not meet the needs of high performance device; Chemical coprecipitation area method easily forms agglomeration, causes distribution of sizes uneven; Sol-gel method length consuming time, post-processing temperature is high; This three kinds of traditional methods or need to introduce other foreign ions, introduce by product, end processing sequences is complicated, or reaction environment is required harsh, need to carry out under high temperature and high pressure environment, cause production cost to strengthen, be difficult to the multivariant oxide nano material with complete crystal formation obtaining meeting stoichiometric ratio, therefore, as how simple and easy method prepares high-quality multi-element metal oxide, be this area technical barrier urgently to be resolved hurrily always.
Summary of the invention
For the problems referred to above, the preparation method of multivariant oxide nano material, the method is simple to operate, and reaction process does not need to introduce additional chemical reagent, environmental protection, and the present invention is achieved in that
A preparation method for multivariant oxide nano material, described nano material has general formula A
xb
yo
z, in formula, A, B are any two kinds in Zn, Ge, Fe, Mn, Ni or Co, and xa+by=2z, a and b are respectively the valence state of metal element A and B; The concrete steps preparing this nano material are as follows:
A two kinds of metal targets immerse in deionized water by () respectively, carry out laser ablation 5-50min respectively with Nd:YAG pulse laser, and metal targets forms colloidal solution; Described metal targets is any two kinds in Zn, Ge, Fe, Mn, Ni or Co;
B two kinds of colloidal solution that step a obtains by (), with after the speed mix and blend 5-10min of 500rpm, move in high-pressure hydrothermal reaction kettle, 80-180 DEG C of thermotonus 2-6h, and the crystallization of reaction gained is described multivariant oxide nano material.
Preferably, in the present invention, describedly carry out laser ablation with Nd:YAG pulse laser and refer to: with wavelength 1064 nanometer, frequency 5-10 hertz, the Nd:YAG pulse laser of pulse energy 100-180 MJ/pulse carries out ablation to metal targets.
Preferably, in the present invention, the beam spot diameter, that in described laser ablation, laser is formed in metal targets is 2 millimeters.
The colloidal solution that the present invention utilizes liquid laser ablation to prepare has greater activity, as the presoma of reaction, rapidly and efficiently obtain the multivariant oxide of well-crystallized under cryogenic, do not need in the method reaction process to introduce any additional substance (as objectionable impuritiess such as the ion in traditional method, soda acids), can not to water body and environment, environmental protection; Meanwhile, by controlling the different ablation time, different colloid output can be obtained, control different hybrid reaction time, temperature, different crystalline nano material can be obtained, in general, mixing temperature is higher, and the reaction times is longer, and material crystalline is better; One aspect of the present invention has widened the application of liquid laser ablation technology in prepared by material, on the other hand also for other ternarys of synthesis or multivariant oxide nano material provide a kind of new thinking.
Accompanying drawing explanation
Fig. 1 is example 1 Zn of the present invention
2geO
4x-ray diffraction spectrogram.
Fig. 2 is example 1 Zn of the present invention
2geO
4electron scanning micrograph.
Fig. 3 is example 2 Zn of the present invention
2snO
4x-ray diffraction spectrogram.
Fig. 4 is example 3 ZnFe of the present invention
2o
4x-ray diffraction spectrogram.
Fig. 5 is example 4 NiCo of the present invention
2o
4x-ray diffraction spectrogram.
Fig. 6 is example 5 FeGe of the present invention
2o
4x-ray diffraction spectrogram.
Fig. 7 is example 6 ZnMnO of the present invention
3x-ray diffraction spectrogram.
Embodiment:
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1 Zn
2geO
4synthesis
By purity be more than 99.99% zinc target be immersed in 24ml deionized water, adopt Nd:YAG pulse laser, wavelength 1064 nanometer, frequency 5-10 hertz, pulse energy 110 MJs/pulse, laser beam transfer optics is 1064 nanometer, 45 degree of high reflective mirrors, laser beam focusing element to be focal length the be convex lens of 20 centimetres, after focusing on, the bundle spot of light beam on target is the circle of diameter 2 millimeters, ablation zinc target 50 minutes, and zinc target forms the metastable nano material colloidal solution of high reactivity hyperergy; By purity be more than 99.99% germanium target be immersed in 22ml deionized water, adopt identical Nd:YAG Pulsed Laser Parameters, ablation germanium target 25 minutes, germanium target forms the metastable nano material colloidal solution of high reactivity hyperergy; By the two kinds of metastable nano material colloidal solution obtained, the speed mix and blend of 500rpm, after 5-10 minute, proceeds in high-pressure hydrothermal reaction kettle, reacts 2 hours, 4 hours and 6 hours at 180 DEG C respectively, namely obtains six good side Zn of crystallinity
2geO
4, Fig. 1 is six obtained side Zn
2geO
4xRD spectra, as seen from the figure, all diffraction peaks are all consistent with standard card, and its good crystallinity is described, do not have the by product of other thing phases to occur, Fig. 2 is gained Zn
2geO
4electron scanning micrograph, as seen from Figure 2, Zn
2geO
4even size distribution, length about 3.5 microns.
Embodiment 2 Zn
2snO
4synthesis
By purity be more than 99.99% zinc target be immersed in 24ml deionized water, adopt Nd:YAG pulse laser, wavelength 1064 nanometer, frequency 5-10 hertz, pulse energy 120 MJs/pulse, ablation zinc target 30 minutes, zinc target forms metastable nano material colloidal solution; Then by purity be more than 99.99% tin target be immersed in 24ml deionized water, adopt same laser parameter, ablation tin target 5 minutes, tin target forms metastable nano material colloidal solution; By two kinds of metastable nano material colloidal solution mix and blend 5-10 minute, proceed in high-pressure hydrothermal reaction kettle, react 6 hours at 180 DEG C, the good Zn of crystallinity
2snO
4, its X-ray diffraction spectrogram as shown in Figure 3.
Embodiment 3 ZnFe
2o
4synthesis
By purity be more than 99.99% zinc target be immersed in 24ml deionized water, adopt Nd:YAG pulse laser, wavelength 1064 nanometer, frequency 5-10 hertz, pulse energy 120 MJs/pulse, ablation zinc target 30 minutes, zinc target forms metastable nano material colloidal solution; Then by purity be more than 99.99% iron target be immersed in 25ml deionized water, adopt parameter be wavelength 1064 nanometer, frequency 5-10 hertz, pulse energy 180 MJs/pulse, ablation iron target 50 minutes, iron target forms metastable nano material colloidal solution; By two kinds of metastable nano material colloidal solution mix and blend 5-10 minute, proceed in high-pressure hydrothermal reaction kettle, react 6 hours at 180 DEG C, the good ZnFe of crystallinity
2o
4, its X-ray diffraction spectrogram as shown in Figure 4.
Embodiment 4 NiCo
2o
4synthesis
By purity be more than 99.99% cobalt target be immersed in 30ml deionized water, adopt Nd:YAG pulse laser, wavelength 1064 nanometer, frequency 5-10 hertz, pulse energy 180 MJs/pulse, ablation cobalt target 30 minutes, cobalt target forms colloidal solution; Then by purity be more than 99.99% nickel target be immersed in 25ml deionized water, adopt same laser parameter, ablation nickel target 15 minutes, nickel target formed colloidal solution; Then two kinds of colloidal solution mix and blends, after 5-10 minute, are proceeded in high-pressure hydrothermal reaction kettle, react 6 hours at 180 DEG C, the good NiCo of crystallinity
2o
4, its X-ray diffraction spectrogram as shown in Figure 5.
Embodiment 5 FeGe
2o
4synthesis
By purity be more than 99.99% iron target be immersed in 25ml deionized water, adopt Nd:YAG pulse laser, wavelength 1064 nanometer, frequency 5-10 hertz, pulse energy 180 MJs/pulse, ablation iron target 50 minutes, iron target forms metastable nano material colloidal solution; Then by purity be more than 99.99% germanium target be immersed in 25ml deionized water, adopt parameter be wavelength 1064 nanometer, frequency 5-10 hertz, pulse energy 110 MJs/pulse, ablation germanium target 25 minutes, the metastable nano material colloidal solution of germanium target; Then two kinds of metastable nano material colloidal solution mix and blends, after 5-10 minute, are proceeded in high-pressure hydrothermal reaction kettle, react 6 hours at 180 DEG C, the good FeGe of crystallinity
2o
4, its X-ray diffraction spectrogram as shown in Figure 6.
Embodiment 6 ZnMnO
3synthesis
Purity be more than 99.99% zinc target be immersed in 24ml deionized water, adopt Nd:YAG pulse laser, wavelength 1064 nanometer, frequency 5-10 hertz, pulse energy 120 MJs/pulse, ablation zinc target 50 minutes, zinc target forms colloidal solution; Then by purity be more than 99.99% manganese target material be immersed in 24ml deionized water, adopt same laser parameter, ablation manganese target material 25 minutes, manganese target material formed colloidal solution; Then two kinds of colloidal solution mix and blends, after 5-10 minute, are proceeded in high-pressure hydrothermal reaction kettle, react 6 hours at 180 DEG C, the good ZnMnO of crystallinity
3, its X-ray diffraction spectrogram as shown in Figure 7.
Embody rule approach of the present invention is a lot, and the above is only the preferred embodiment of the present invention, should be understood that; for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvement, these improvement also should be considered as protection scope of the present invention.
Claims (3)
1. a preparation method for multivariant oxide nano material, is characterized in that, described nano material has general formula A
xb
yo
z, in formula, A, B are any two kinds in Zn, Ge, Fe, Mn, Ni or Co, and xa+by=2z, a and b are respectively the valence state of metal element A and B; The concrete steps preparing this nano material are as follows:
A two kinds of metal targets immerse in deionized water by () respectively, carry out laser ablation 5-50min respectively with Nd:YAG pulse laser, and metal targets forms colloidal solution; Described metal targets is any two kinds in Zn, Ge, Fe, Mn, Ni or Co;
B two kinds of colloidal solution that step a obtains by (), with after the speed mix and blend 5-10min of 500rpm, move in high-pressure hydrothermal reaction kettle, 80-180 DEG C of thermotonus 2-6h, and the crystallization of reaction gained is described multivariant oxide nano material.
2. the preparation method of multivariant oxide nano material according to claim 1, it is characterized in that, describedly carry out laser ablation with Nd:YAG pulse laser and refer to: with wavelength 1064 nanometer, frequency 5-10 hertz, the Nd:YAG pulse laser of pulse energy 100-180 MJ/pulse carries out ablation to metal targets.
3. the preparation method of multivariant oxide nano material according to claim 2, it is characterized in that, the beam spot diameter, that in described laser ablation, laser is formed in metal targets is 2 millimeters.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106629821A (en) * | 2016-09-12 | 2017-05-10 | 南京理工大学 | Method for preparing submicron metal hydroxystannate ZnSn(OH)6 cube block |
| CN107758726A (en) * | 2017-09-30 | 2018-03-06 | 南京理工大学 | One kind can be used for deep ultraviolet pole weak light detection high-purity nm structure ZnGa2O4Preparation method |
| CN109292821A (en) * | 2018-10-18 | 2019-02-01 | 合肥学院 | A kind of monocrystalline TT-Nb2O5The preparation method of nano-pillar |
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| US20040080339A1 (en) * | 2002-10-23 | 2004-04-29 | Mitsubishi Denki Kabushiki Kaisha | Semiconductor device with bus terminating function |
| CN101327946A (en) * | 2008-06-05 | 2008-12-24 | 中山大学 | Micro-nanoparticle having special morphology, preparation and use thereof |
| CN101798115A (en) * | 2010-02-26 | 2010-08-11 | 中山大学 | Preparation method of ternary oxysalt compound micro-nano material |
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2015
- 2015-01-05 CN CN201510002382.6A patent/CN104528807A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040080339A1 (en) * | 2002-10-23 | 2004-04-29 | Mitsubishi Denki Kabushiki Kaisha | Semiconductor device with bus terminating function |
| CN101327946A (en) * | 2008-06-05 | 2008-12-24 | 中山大学 | Micro-nanoparticle having special morphology, preparation and use thereof |
| CN101798115A (en) * | 2010-02-26 | 2010-08-11 | 中山大学 | Preparation method of ternary oxysalt compound micro-nano material |
Non-Patent Citations (1)
| Title |
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| SHOULIANG WU等: "Reduced graphene oxide anchored magnetic ZnFe2O4 nanoparticles with enhanced visible-light photocatalytic activity", 《RSC ADV.》, 22 December 2014 (2014-12-22), pages 9069 - 9074 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106629821A (en) * | 2016-09-12 | 2017-05-10 | 南京理工大学 | Method for preparing submicron metal hydroxystannate ZnSn(OH)6 cube block |
| CN107758726A (en) * | 2017-09-30 | 2018-03-06 | 南京理工大学 | One kind can be used for deep ultraviolet pole weak light detection high-purity nm structure ZnGa2O4Preparation method |
| CN107758726B (en) * | 2017-09-30 | 2019-10-18 | 南京理工大学 | One kind can be used for deep ultraviolet pole weak light detection high-purity nm structure ZnGa2O4Preparation method |
| CN109292821A (en) * | 2018-10-18 | 2019-02-01 | 合肥学院 | A kind of monocrystalline TT-Nb2O5The preparation method of nano-pillar |
| CN109292821B (en) * | 2018-10-18 | 2021-01-26 | 合肥学院 | Monocrystal TT-Nb2O5Preparation method of nano-column |
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Application publication date: 20150422 |