CN103011307A - Method for synthesizing NiO nanocube particles through milisecond pulsed laser - Google Patents
Method for synthesizing NiO nanocube particles through milisecond pulsed laser Download PDFInfo
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- CN103011307A CN103011307A CN2012105757875A CN201210575787A CN103011307A CN 103011307 A CN103011307 A CN 103011307A CN 2012105757875 A CN2012105757875 A CN 2012105757875A CN 201210575787 A CN201210575787 A CN 201210575787A CN 103011307 A CN103011307 A CN 103011307A
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Abstract
The invention relates to a method for synthesizing NiO nanocube particles through a milisecond pulsed laser. The method realizes the preparation of lots of NiO nanocube particles under a room temperature condition; and the prepared products have high purity. The method comprises the steps of taking micron-level metallic nickel powder as a raw material, and dispersing the micron-order metallic nickel powder in a deionized water to form a mixture; using a submerged pump to enable the metallic nickel powder and water mixture to ceaselessly circulate; using the milisecond pulsed laser to bombard a circulating deionized water medium containing the metallic nickel powder; and purifying the product bombarded by the milisecond pulsed laser to obtain the NiO nanocube particles. The method realizes the synthesis of the NiO nanocube particles at normal temperature and pressures, and the NiO nanocube particles with higher purity are obtained at high efficiency by adopting the method.
Description
Technical field
The invention relates to nano material, relate in particular to the method for the synthetic NiO nanocubes particle of a kind of millisecond of pulse laser.
Background technology
NiO nanocubes particle is a kind of nano material with regular cubes pattern that is formed by the nickel oxide with face-centred cubic structure.Because the outside surface that NiO nanocubes particle is exposed has greater activity, greatly expanded the range of application of NiO nanocubes particulate material, made it demonstrate huge potential using value in many science and technology field such as catalysis, Novel lithium battery electrode materialss.
NiO nanocubes particulate material is as a kind of novel nano-material, and the research of its preparation, performance and application has become the study hotspot of material science.At present, the method for preparing NiO nanocubes particulate material mainly is the pure metallic nickel target in the femtosecond laser ablation enclosed housing---a small amount of NiO nanocubes particle adopted the pure metallic nickel target in the femtosecond laser ablation nickel high vacuum seal cavity to observe by U.S. Yong Che group in 2007, but NiO nanocubes particle only is to follow nano nickel particles and the by product that produces, referring to Liu et al, applied physics letters, 2007,90:044103.This method is under the condition of high vacuum degree environment, ablates by metallic nickel target with femtosecond laser beam, and in the ablation process, the cathode bias ion probe is placed on nickel target the place ahead and collects product.Adopt at present the method can obtain the NiO nanocubes particle of the less and narrow distribution of size, but owing to reaction conditions is required comparatively harsh, and product mainly is comprised of nano nickel particles, NiO nanocubes particle occurs as just by product, the output of NiO nanocubes particle is extremely low, the comparison in equipment of this method use is complicated in addition, processing parameter is wayward, power consumption is large, cost is high, is difficult to realize extensive synthetic.
Summary of the invention
Purpose of the present invention, to prepare in the technique of NiO nanocubes particle the wayward and problem such as product purity is low, output is little of reaction conditions for prior art, utilize the millisecond pulsed laser technique to prepare the advantage of nano material, a kind of and reactant long duration of action are provided, and technique is simple and can prepare in a large number the novel method of NiO nanocubes particle under normal temperature and pressure conditions.
The method of the synthetic NiO nanocubes particle of millisecond pulse laser provided by the invention has following steps:
The method of a kind of millisecond of synthetic NiO nanocubes particle of pulse laser has following steps:
(a) the micron order metallic nickel powder is mixed with water, utilize submersible pump to make its constantly circulation dispersion in reaction;
(b) metallic nickel powder in the use pulse laser bombardment recirculated water, wherein laser spot converges under the fluid surface of metallic nickel powder suspension, laser output wavelength 1064nm, power density 10
6～10
7W/cm2, pulsewidth 0.6～1.0ms, the pulse laser beam of frequency 10～20Hz, laser beam focus on following approximately 1～2mm place, liquid medium surface, and spot size is 0.2～0.3mm approximately, and the time of lasing is at 4 ~ 10h;
(c) product after the laser bombardment is obtained NiO nanocubes particle through simply leaving standstill, purifying;
The method of purification of step (c) is:
(1) removes the larger nickel particle of particle diameter
It is in the 10-20 deionized water doubly that the mixture that comprises NiO nanocubes product that laser method is synthetic joins mass ratio, stirred 5 minutes under the normal temperature, utilize aperture size between 0.250mm-0.125mm, it is the filtering net filtration between the 60-120 order, remove the larger nickel particle of particle diameter in the product, obtain first purified product;
(2) remove the less nickel particle of particle diameter
The purified product adding mass ratio that step (1) is obtained is in the 2-4 deionized water doubly, at normal temperatures, utilize the agitator stirring at low speed, in container, place simultaneously the less nickel particle of particle diameter in the magnet adsorption solution, stir after 5 minutes, take out magnet, manually scrape off the material that adsorbs on the magnet; And then magnet is placed in the container, continue to stir 5 minutes, take out magnet, scrape off again adsorbent on the magnet; Three times and so forth;
(3) moisture is removed in cryodrying
Remaining liq in step (2) container is taken out, and moisture was removed in cryodrying in 24 hours, obtained high purity N iO nanocubes particle.
Particle diameter 45～55 μ m of the micron order metallic nickel powder of described step (a).
The present invention has overcome prior art and has prepared the deficiency that reaction conditions is wayward, conversion unit is expensive, product purity is low, output is few in the technique of NiO nanocubes particle, realize at normal temperatures and pressures synthesizing of NiO nanocubes particle, obtained the higher NiO nanocubes particle of purity.In addition, synthetic method of the present invention has the advantages such as technique is simple, reaction process safety NiO nanocubes particle size distribution controlled, that obtain is even.
Description of drawings
Fig. 1 is the laser irradiation suspension device schematic diagram of the synthetic NiO nanocubes particle of preparation millisecond pulse laser of the present invention;
Fig. 2 is the transmission electron microscope shape appearance figure of the synthetic NiO nanocubes particle of 2 milliseconds of pulse lasers of embodiment.
Reference numeral among Fig. 1 is:
1---Nd:YAG laser apparatus 2---pulse laser
3---metallic nickel powder and water mixture 4---submersible pump
Embodiment
The present invention adopts the laser irradiation suspension device of the synthetic NiO nanocubes particle of the preparation of Fig. 1 millisecond pulse laser of the present invention, and this device is comprised of Nd:YAG laser apparatus 1, pulse laser 2, metallic nickel powder loop suspension 3, submersible pump 4.The focus of pulse laser 2 is converged at 1～2mm below the liquid level of metallic nickel powder suspension 3, the particle in the metallic nickel powder suspension 3 disperses by submersible pump 4 recirculated waters.
By Nd-YAG solid statelaser output wavelength 1064nm, power density 10
6W/cm2, pulsewidth 0.6ms, the pulse laser beam of frequency 10Hz, laser beam focus on following approximately 1mm place, liquid medium surface, and spot size is 0.2mm approximately.
Be that 50 μ m metallic nickel powders mix with deionized water with particle diameter, utilize submersible pump make its in reaction constantly circulation disperse.
Use the metallic nickel powder in the millisecond pulse laser bombardment water, laser spot converges at the suitable distance in underwater, produced the microcell of a High Temperature High Pressure at the laser spot place, impelled the metallic nickel particle gasification in the microcell and then in the process of condensation, form NiO nanocubes particle.The laser power density of the zone of action is 10
6W/cm
2, the time of lasing is at 10h.
Wherein: metallic nickel powder should be in water Uniform Dispersion.Because submersible pump is to the dissemination of mixed powder, so that millisecond laser acts on different metallic nickel particles constantly in difference, be conducive to improve preparation efficiency.
To the product after the laser bombardment through simply leaving standstill, purify the NiO nanocubes particle that obtains grey.Size distribution is between 10 ~ 40nm.
By Nd-YAG solid statelaser output wavelength 1064nm, power density 10
7W/cm2, pulsewidth 1.0ms, the pulse laser beam of frequency 20Hz, laser beam focus on following approximately 2mm place, liquid medium surface, and spot size is 0.3mm approximately.
Be that 45 μ m metallic nickel powders mix with deionized water with particle diameter, utilize submersible pump make its in reaction constantly circulation disperse.
Use the metallic nickel powder in the millisecond pulse laser bombardment water, laser spot converges at the suitable distance in underwater, produced the microcell of a High Temperature High Pressure at the laser spot place, impelled the metallic nickel particle gasification in the microcell and then in the process of condensation, form NiO nanocubes particle.The laser power density of the zone of action is 10
7W/cm
2, the time of lasing is at 5h.
Wherein: metallic nickel powder should be in water Uniform Dispersion.Because submersible pump is to the dissemination of mixed powder, so that millisecond laser acts on different metallic nickel particles constantly in difference, be conducive to improve preparation efficiency.
With reacted product through leave standstill and separating-purifying after obtain the NiO nanocubes particle of grey, size distribution is between 10 ~ 40nm.Referring to Fig. 2, be the millisecond pulse laser bombardment metal nickel powder of the present embodiment and the NiO nanocubes particle transmission electron microscope photo of water mixture preparation shown in the figure, as can be seen from the figure the size of NiO nanocubes particle is between 10 ~ 40nm, the well-regulated square pattern of most of particle tools.
Claims (2)
1. the method for the synthetic NiO nanocubes particle of a millisecond pulse laser has following steps:
(a) the micron order metallic nickel powder is mixed with water, utilize submersible pump to make its constantly circulation dispersion in reaction;
(b) metallic nickel powder in the use pulse laser bombardment recirculated water, wherein laser spot converges under the fluid surface of metallic nickel powder suspension, laser output wavelength 1064nm, power density 10
6～10
7W/cm2, pulsewidth 0.6～1.0ms, the pulse laser beam of frequency 10～20Hz, laser beam focus on following approximately 1～2mm place, liquid medium surface, and spot size is 0.2～0.3mm approximately, and the time of lasing is at 4 ~ 10h;
(c) product after the laser bombardment is obtained NiO nanocubes particle through simply leaving standstill, purifying;
The method of purification of step (c) is:
(1) removes the larger nickel particle of particle diameter
It is in the 10-20 deionized water doubly that the mixture that comprises NiO nanocubes product that laser method is synthetic joins mass ratio, stirred 5 minutes under the normal temperature, utilize aperture size between 0.250mm-0.125mm, it is the filtering net filtration between the 60-120 order, remove the larger nickel particle of particle diameter in the product, obtain first purified product;
(2) remove the less nickel particle of particle diameter
The purified product adding mass ratio that step (1) is obtained is in the 2-4 deionized water doubly, at normal temperatures, utilize the agitator stirring at low speed, in container, place simultaneously the less nickel particle of particle diameter in the magnet adsorption solution, stir after 5 minutes, take out magnet, manually scrape off the material that adsorbs on the magnet; And then magnet is placed in the container, continue to stir 5 minutes, take out magnet, scrape off again adsorbent on the magnet; Three times and so forth;
(3) moisture is removed in cryodrying
Remaining liq in step (2) container is taken out, and moisture was removed in cryodrying in 24 hours, obtained high purity N iO nanocubes particle.
2. according to claim 1 the method for the synthetic NiO nanocubes particle of millisecond pulse laser is characterized in that particle diameter 45～55 μ m of the micron order metallic nickel powder of described step (a).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108640135A (en) * | 2018-07-17 | 2018-10-12 | 郑强 | A kind of nanometer spherical high purity aluminium oxide process for cleanly preparing |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1493526A (en) * | 2003-09-16 | 2004-05-05 | 上海大学 | Collosol gel production method of nano NiO material |
| CN102134106A (en) * | 2011-03-09 | 2011-07-27 | 绍兴文理学院 | Method for preparing beta-nickel hydroxide with different shapes |
| US20120128996A1 (en) * | 2008-09-12 | 2012-05-24 | Lg Chem Ltd | Metal nanobelt and method of manufacturing the same, and conductive ink composition and conductive film comprising the same |
-
2012
- 2012-12-26 CN CN2012105757875A patent/CN103011307A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1493526A (en) * | 2003-09-16 | 2004-05-05 | 上海大学 | Collosol gel production method of nano NiO material |
| US20120128996A1 (en) * | 2008-09-12 | 2012-05-24 | Lg Chem Ltd | Metal nanobelt and method of manufacturing the same, and conductive ink composition and conductive film comprising the same |
| CN102134106A (en) * | 2011-03-09 | 2011-07-27 | 绍兴文理学院 | Method for preparing beta-nickel hydroxide with different shapes |
Non-Patent Citations (1)
| Title |
|---|
| 田飞等: "毫秒脉冲激光辐照炭黑颗粒悬浮液制备纳米金刚石", 《金刚石与磨料磨具工程》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108640135A (en) * | 2018-07-17 | 2018-10-12 | 郑强 | A kind of nanometer spherical high purity aluminium oxide process for cleanly preparing |
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Application publication date: 20130403 |