CN104308166A - Method for preparing Ag/ZnO core-shell nanostructure by adopting pulse laser liquid ablation - Google Patents
Method for preparing Ag/ZnO core-shell nanostructure by adopting pulse laser liquid ablation Download PDFInfo
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- CN104308166A CN104308166A CN201410532570.5A CN201410532570A CN104308166A CN 104308166 A CN104308166 A CN 104308166A CN 201410532570 A CN201410532570 A CN 201410532570A CN 104308166 A CN104308166 A CN 104308166A
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Abstract
The invention discloses a method for preparing an Ag/ZnO core-shell nanostructure by adopting pulse laser liquid ablation and belongs to the field of material preparation. Two-step pulse laser liquid ablation is adopted, oxide layers of an Ag target and a Zn target are removed by using nitric acid, and ultrasonic cleaning is performed. The method comprises the following steps of ablating the Ag target in deionized water by using excimer laser with the wavelength of 248nm, the single pulse energy of 400mJ and the repetition frequency of 10Hz to obtain Ag colloid; ablating the Zn target in the Ag colloid by using the same laser to obtain the Ag/ZnO core-shell nanostructure. According to the method, preparation equipment is simple, the preparation is quick and safe without pollution, the surface plasma resonance absorption of the prepared Ag/ZnO core-shell nanostructure can be adjusted, and the Ag/ZnO core-shell nanostructure has other excellent photoelectric properties and has a good application prospect in the fields of optics, electrics, catalysis and the like.
Description
Technical field
The invention belongs to field of material preparation.
Background technology
Strong coupling effect is there is between precious metal surface Resonance Plasma and semiconductor exciton, especially be the performance that the nucleocapsid structure of representative shows many uniquenesses in electricity, optics, catalysis with Ag/ZnO, at micro-nano field of photoelectric devices, there is huge application potential.Up to the present the article of a lot of preparation Ag/ZnO nanometer nuclear shell nano-structure is had, but be all the chemical synthesis adopted, chemical synthesis has technical maturity, hold manageable feature, but chemical synthesis inevitably introduces some impurity in preparation process, which greatly limits the application of chemical method synthesis Ag/ZnO product.Pulse laser liquid phase ablation is a kind of simple, and fast, the green method preparing nano material, employing pulse laser ablation is in the metal targets in liquid phase environment, obtains the nano-scale particle disperseed in a liquid.Have synthesis device simple, preparation fast, does not have the feature that impurity is introduced in preparation process.
Summary of the invention
The object of the present invention is to provide one to prepare simply, fast, in preparation process, there is no the method preparing Ag/ZnO nanometer nuclear shell nano-structure that impurity is introduced.
The object of the invention is to be achieved through the following technical solutions:
1) successively clean at absolute ethyl alcohol and deionized water for ultrasonic after carrying out machine glazed finish also after Ag target and Zn target nitric acid being removed oxide layer.
2) the Ag target cleaned is positioned over the beaker bottom that deionized water is housed, beaker is positioned on rotation platform, rotary speed 10-60 rev/min.Be 248nm with wavelength, the KrF PRK of single pulse energy 400mJ, repetition rate 10Hz focuses on Ag target surface after reflection to Ag target ablation 10-30 minute.
3) take out Ag target, Zn target is positioned over the Ag colloid prepared, beaker is positioned on rotation platform, rotary speed 10-60 rev/min.Employing wavelength is 248nm, and KrF PRK ablation 5-20 minute under oxygen atmosphere of single pulse energy 400mJ, repetition rate 10Hz, obtains the nano-particle colloid of Ag/ZnO nucleocapsid structure.
2. the above adopts laser liquid phase ablation to prepare the method for Ag/ZnO nanometer nuclear shell nano-structure, it is characterized in that the metallic target adopted eliminates surface oxide layer, and surface is through machine glazed finish.
3. the above adopts laser liquid phase ablation to prepare the method for Ag/ZnO nanometer nuclear shell nano-structure, it is characterized in that said laser instrument is KrF excimer laser, laser parameter: wavelength 248nm, single pulse energy 400mJ, repetition rate 10Hz, ablation first stage, 10-30 minute time, second stage ablation time 5-20 minute.
4. the above adopts laser liquid phase ablation to prepare the method for Ag/ZnO nanometer nuclear shell nano-structure, it is characterized in that the rotating speed of adopted rotation platform is 10-60 rev/min.
5. the above adopts laser liquid phase ablation to prepare the method for Ag/ZnO nanometer nuclear shell nano-structure, it is characterized in that ablation Zn target carries out under 0.5-2 atmospheric oxygen atmosphere.
The present invention is owing to taking above technical scheme, and it has the following advantages:
1. to prepare its technological operation of Ag/ZnO nanometer nuclear shell nano-structure simple for pulse laser liquid phase ablation, and manufacturing cycle is short, in preparation process, do not introduce impurity.
2. the surfaces of the Ag/ZnO nanometer nuclear shell nano-structure prepared etc. can by controlling ablation time controling from resonance.
3. the purer ZnO of ultra-violet light-emitting of the Ag/ZnO nanometer nuclear shell nano-structure prepared has very large enhancing, and band gap width increases to some extent.
Accompanying drawing explanation
Fig. 1 is the ablation device schematic diagram that the present invention uses.
1 PRK 2 speculum 3 lens supports
4 focus lamp 5 quartz window 6 beakers
7 ablation target 8 adjustable speed rotation platform 9 carrier bases
Fig. 2 is the transmission electron microscope image of Ag/ZnO nanometer nuclear shell nano-structure.
Fig. 3 is the XRD diffracting spectrum of Ag/ZnO nanometer nuclear shell nano-structure.
Fig. 4 is the change of surface plasma body resonant vibration light absorption with the ablation time of Ag/ZnO nanometer nuclear shell nano-structure.
Fig. 5 is that the Ag/ZnO nanometer nuclear shell nano-structure of embodiment 1 preparation and the photoluminescence spectrum of pure ZnO contrast.
Fig. 6 is that the Ag/ZnO nanometer nuclear shell nano-structure of embodiment 2 preparation and the photoluminescence spectrum of pure ZnO contrast.
Fig. 7 is that the Ag/ZnO nanometer nuclear shell nano-structure of embodiment 3 preparation and the photoluminescence spectrum of pure ZnO contrast.
Fig. 8 is that the Ag/ZnO nanometer nuclear shell nano-structure of embodiment 4 preparation and the photoluminescence spectrum of pure ZnO contrast.
Detailed description of the invention
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
Embodiment 1:
Ag target and Zn target are first removed surface oxide layer in 1 minute with nitric acid dousing, by the fine sandpaper machine glazed finish of Ag and Zn target, Ag and the Zn of polishing metallic target is successively ultrasonic with supersonic cleaning machine in absolute ethyl alcohol and deionized water.The ablation device adopted in experiment as shown in Figure 1.The Ag target cleaned is positioned over the beaker bottom that 10ml deionized water is housed, beaker is positioned on rotation platform, rotary speed 10 revs/min.Ag target surface is focused on after reflection to Ag target ablation 30 minutes with the KrF PRK (single pulse energy 400mJ, repetition rate 10Hz) that wavelength is 248nm.Take out Ag target, Zn target is positioned in the Ag colloid prepared, beaker is positioned on rotation platform, rotary speed 10 revs/min.Adopt identical laser parameter (wavelength 248nm, single pulse energy 400mJ, repetition rate 10Hz) under 1 atmospheric oxygen, carry out ablation 20 minutes, obtain the dispersion colloid of Ag/ZnO nanometer nuclear shell nano-structure.
Fig. 2 is the transmission electron microscope image being in the Ag/ZnO nanometer nuclear shell nano-structure on copper mesh adopting high resolution transmission electron microscopy to irradiate.Obviously can find out that from figure product is nucleocapsid structure, core is of a size of 10nm, and thickness of the shell is about 5nm.And can find out that from full resolution pricture core be Ag shell is ZnO.
Fig. 3 is the XRD diffracting spectrum of Ag/ZnO nanometer nuclear shell nano-structure prepared by the method.As can be seen from the figure, all peak positions all belong to Ag and ZnO, do not have other peaks to occur, illustrate and do not have impurity to introduce.Ag occurs with the form of elemental silver metal, illustrates that Ag is not oxidized in preparation process.
Fig. 4 is the Ultraviolet visible absorption spectrum of the Ag/ZnO nanometer nuclear shell nano-structure prepared of the method and Ag nano particle, can obviously find out from figure, the optical absorption peak of Ag/ZnO nanometer nuclear shell nano-structure has very large red shift than Ag nano particle, illustrates that Ag/ZnO nucleocapsid structure creates larger impact on the surface of Ag etc. from resonance.
Fig. 5 is ZnO nano particle photoluminescence spectrum prepared by the Ag/ZnO nanometer nuclear shell nano-structure prepared of the method and laser ablation method, as can be seen from the figure, the ultra-violet light-emitting of Ag/ZnO nanometer nuclear shell nano-structure strengthens to some extent than ZnO nano particle, simultaneously the ultra-violet light-emitting of Ag/ZnO nanometer nuclear shell nano-structure is than the ultra-violet light-emitting blue shift of ZnO nano particle, illustrate that Ag/ZnO nucleocapsid structure enhances the ultra-violet light-emitting effect of ZnO, Ag/ZnO nucleocapsid structure have impact on the energy gap of ZnO simultaneously.
Embodiment 2:
Ag target and Zn target are first removed surface oxide layer in 1 minute with nitric acid dousing, by the fine sandpaper machine glazed finish of Ag and Zn target, Ag and the Zn of polishing metallic target is successively ultrasonic with supersonic cleaning machine in absolute ethyl alcohol and deionized water.The ablation device adopted in experiment as shown in Figure 1.The Ag target cleaned is positioned over the beaker bottom that 10ml deionized water is housed, beaker is positioned on rotation platform, rotary speed 15 revs/min.Ag target surface is focused on after reflection to Ag target ablation 20 minutes with the KrF PRK (single pulse energy 400mJ, repetition rate 10Hz) that wavelength is 248nm.Take out Ag target, Zn target is positioned in the Ag colloid prepared, beaker is positioned on rotation platform, rotary speed 15 revs/min.Adopt identical laser parameter (wavelength 248nm, single pulse energy 400mJ, repetition rate 10Hz) under 1 atmospheric oxygen, carry out ablation 5 minutes, obtain another group Ag/ZnO nanometer nuclear shell nano-structure.
Fig. 6 is the Ultraviolet visible absorption spectrum of the Ag/ZnO nanometer nuclear shell nano-structure prepared of the method and Ag nano particle, can obviously find out from figure, the optical absorption peak of Ag/ZnO nanometer nuclear shell nano-structure has very large red shift than Ag nano particle, illustrates that Ag/ZnO nucleocapsid structure creates larger impact on the surface of Ag etc. from resonance.
Embodiment 3:
Ag target and Zn target are first removed surface oxide layer in 1 minute with nitric acid dousing, by the fine sandpaper machine glazed finish of Ag and Zn target, Ag and the Zn of polishing metallic target is successively ultrasonic with supersonic cleaning machine in absolute ethyl alcohol and deionized water.The ablation device adopted in experiment as shown in Figure 1.The Ag target cleaned is positioned over the beaker bottom that 10ml deionized water is housed, beaker is positioned on rotation platform, rotary speed 30 revs/min.Ag target surface is focused on after reflection to Ag target ablation 20 minutes with the KrF PRK (single pulse energy 400mJ, repetition rate 10Hz) that wavelength is 248nm.Take out Ag target, Zn target is positioned in the Ag colloid prepared, beaker is positioned on rotation platform, rotary speed 30 revs/min.Adopt identical laser parameter (wavelength 248nm, single pulse energy 400mJ, repetition rate 10Hz) under 1 atmospheric oxygen, carry out ablation 10 minutes, obtain another group Ag/ZnO nanometer nuclear shell nano-structure.
Fig. 7 is the Ultraviolet visible absorption spectrum of the Ag/ZnO nanometer nuclear shell nano-structure prepared of the method and Ag nano particle, can obviously find out from figure, the optical absorption peak of Ag/ZnO nanometer nuclear shell nano-structure has very large red shift than Ag nano particle, illustrates that Ag/ZnO nucleocapsid structure creates larger impact on the surface of Ag etc. from resonance.
Embodiment 4:
Ag target and Zn target are first removed surface oxide layer in 1 minute with the nitric acid dousing of 30%, by the fine sandpaper machine glazed finish of Ag and Zn target, Ag and the Zn of polishing metallic target is successively ultrasonic with supersonic cleaning machine in absolute ethyl alcohol and deionized water.The ablation device adopted in experiment as shown in Figure 1.The Ag target cleaned is positioned over the beaker bottom that 10ml deionized water is housed, beaker is positioned on rotation platform, rotary speed 60 revs/min.Ag target surface is focused on after reflection to Ag target ablation 30 minutes with the KrF PRK (single pulse energy 400mJ, repetition rate 10Hz) that wavelength is 248nm.Take out Ag target, Zn target is positioned in the Ag colloid prepared, beaker is positioned on rotation platform, rotary speed 60 revs/min.Adopt identical laser parameter (wavelength 248nm, single pulse energy 400mJ, repetition rate 10Hz) under 1 atmospheric oxygen, carry out ablation 15 minutes, obtain another group Ag/ZnO nanometer nuclear shell nano-structure.
Fig. 8 is the Ultraviolet visible absorption spectrum of the Ag/ZnO nanometer nuclear shell nano-structure prepared of the method and Ag nano particle, can obviously find out from figure, the optical absorption peak of Ag/ZnO nanometer nuclear shell nano-structure has very large red shift than Ag nano particle, illustrates that Ag/ZnO nucleocapsid structure creates larger impact on the surface of Ag etc. from resonance.
Claims (3)
1. adopt laser liquid phase ablation to prepare a method for Ag/ZnO nanostructured, it is characterized in that comprising the following steps:
1) successively clean at absolute ethyl alcohol and deionized water for ultrasonic after carrying out machine glazed finish also after Ag target and Zn target nitric acid being removed oxide layer;
2) the Ag target cleaned is positioned over the beaker bottom of deionized water, is positioned over by beaker on rotation platform, rotation platform rotates; With the KrF PRK that wavelength is 248nm, single pulse energy 400mJ, repetition rate 10Hz; Focus on Ag target surface after reflection to Ag target ablation 10-30 minute;
3) take out Ag target, Zn target is positioned over the Ag colloid prepared, beaker is positioned on rotation platform; Adopt identical laser parameter, wavelength 248nm, single pulse energy 400mJ, repetition rate 10Hz, ablation 5-20 minute under oxygen atmosphere, obtains the nano-particle colloid of Ag/ZnO nucleocapsid structure.
2. adopt laser liquid phase ablation to prepare the method for Ag/ZnO nanometer nuclear shell nano-structure according to claim 1, it is characterized in that the rotating speed of adopted rotation platform be 10-60 rev/min adjustable.
3. adopt laser liquid phase ablation to prepare the method for Ag/ZnO nanometer nuclear shell nano-structure according to claim 1, it is characterized in that said ablation is carried out under 0.5-2 atmospheric pressure pure oxygen atmosphere.
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| CN105478791A (en) * | 2015-12-01 | 2016-04-13 | 中国科学院合肥物质科学研究院 | Composite nanometer material with palladium coated with aluminum oxide and preparing method of composite nanometer material |
| CN105689727A (en) * | 2016-01-29 | 2016-06-22 | 中国工程物理研究院流体物理研究所 | Method for preparing solid-dissolved high-bactericidal-activity nanometer Ag-Cu alloy powder by means of in-liquid pulse energy technology |
| CN107052330A (en) * | 2016-10-27 | 2017-08-18 | 中国科学院地球化学研究所 | A kind of method that nanometer metallic iron is obtained and wrapped up |
| CN108423709A (en) * | 2018-01-19 | 2018-08-21 | 南京理工大学 | A kind of ablative method of the device based on double-pulse laser liquid phase ablation synthesizing nanocrystalline |
| CN109529883A (en) * | 2018-11-13 | 2019-03-29 | 北京工业大学 | A method of Cd/S core-shell nanostructure is prepared using pulse laser liquid phase ablation |
| CN110201676A (en) * | 2019-06-21 | 2019-09-06 | 西北工业大学 | A kind of bismuthic acid Copper thin film that inlaying no ligand quantum dot, preparation method and application |
| CN113560712A (en) * | 2021-07-14 | 2021-10-29 | 北京理工大学 | Method for preparing two-dimensional material nanostructure by ultrafast laser processing |
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Cited By (11)
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| CN105478791A (en) * | 2015-12-01 | 2016-04-13 | 中国科学院合肥物质科学研究院 | Composite nanometer material with palladium coated with aluminum oxide and preparing method of composite nanometer material |
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| CN105689727B (en) * | 2016-01-29 | 2017-10-03 | 中国工程物理研究院流体物理研究所 | The method that pulsed power technology prepares high bactericidal properties nanometer Ag Cu alloyed powders |
| CN107052330A (en) * | 2016-10-27 | 2017-08-18 | 中国科学院地球化学研究所 | A kind of method that nanometer metallic iron is obtained and wrapped up |
| CN107052330B (en) * | 2016-10-27 | 2019-01-04 | 中国科学院地球化学研究所 | A kind of method that nanometer metallic iron is obtained and wrapped up |
| CN108423709A (en) * | 2018-01-19 | 2018-08-21 | 南京理工大学 | A kind of ablative method of the device based on double-pulse laser liquid phase ablation synthesizing nanocrystalline |
| CN108423709B (en) * | 2018-01-19 | 2020-03-20 | 南京理工大学 | Ablation method of device for synthesizing nanocrystalline based on double-pulse laser liquid phase ablation |
| CN109529883A (en) * | 2018-11-13 | 2019-03-29 | 北京工业大学 | A method of Cd/S core-shell nanostructure is prepared using pulse laser liquid phase ablation |
| CN110201676A (en) * | 2019-06-21 | 2019-09-06 | 西北工业大学 | A kind of bismuthic acid Copper thin film that inlaying no ligand quantum dot, preparation method and application |
| CN113560712A (en) * | 2021-07-14 | 2021-10-29 | 北京理工大学 | Method for preparing two-dimensional material nanostructure by ultrafast laser processing |
| CN113560712B (en) * | 2021-07-14 | 2022-11-25 | 北京理工大学 | Method for preparing two-dimensional material nanostructure through ultrafast laser processing |
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