CN104014800B - Utilize the preparation method of laser controlledly synthesis single dispersing active metal nano particle - Google Patents
Utilize the preparation method of laser controlledly synthesis single dispersing active metal nano particle Download PDFInfo
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Abstract
The invention discloses and a kind ofly utilize the method for laser controlledly synthesis single dispersing active metal nano particle: take pure metal targets as raw material, again the target handled well is put into laser irradiating device, pass into argon gas, add cyclohexane again, and add oleic acid, make 0.05% < oleic acid volume solubility < 0.12%; Adopt ns focused pulse laser ablation target, obtained simple metal nano-sized colloidal solution; Shift above-mentioned colloidal solution again in another laser irradiating device, the oleic acid volumetric concentration in adjustable ring hexane is 0.14% ~ 0.17%; Employing nanosecond, parallel pulse laser carried out irradiation to metal nano colloidal solution, the single dispersing active metal nano particle of obtained 5 ~ 20nm.Pattern unification is achieved and the controlledly synthesis of the active nano particle of Size Distribution degree < 10% in the present invention's liquid phase at normal temperatures and pressures; The method technique is simple, easy to operate, no coupling product and impurity, is green synthesis process, is suitable for synthesizing most of active metals nano particle.
Description
Technical field
The invention relates to metal nanoparticle, the laser method that particularly a kind of size is controlled synthesizes the preparation method of monodispersed active metal nano particle.
Background technology
Active metal nano particle possesses skin effect specific to nano material and quantum size effect, different in kind is in traditional bulk metal, have a high potential in fields such as catalysis, photoelectricity conduction, information storage and magnetic fluids, have unique using value and wide application prospect.Such as, the magnetic nanoparticles such as iron, cobalt, nickel have been widely used in the biomedical aspects such as target medicine carrier, magnetic thermotherapy, immunoassay, radio-immunity mark, see PankhurstQA, ConnollyJ, JonesSK, etal.Applicationsofmagneticnanoparticlesinbiomedicine [J] .JournalofphysicsD:Appliedphysics, 2003,36 (13): R167.Simultaneously, the physicochemical properties such as optical, electrical, the magnetic of nano particle and its size and pattern closely bound up, very responsive to change in size, can along with the change generation marked change of grain diameter, see PuntesVF, KrishnanKM, AlivisatosAP.Colloidalnanocrystalshapeandsizecontrol:the caseofcobalt [J] .Science, 2001,291 (5511): 2115-2117.Therefore, prepare the active metal nano particle of single dispersing (i.e. pattern unification, good dispersion, Size Distribution degree < 10%) and realize that meaning is had to the regulation and control of its size.
Due to the existence of the problems such as activity is high, oxidizable, easy reunion, synthesis active metal nano particle relative difficult.Current, conventional preparation method is mainly divided into Physical and the large class of chemical method two.Full-fledged with the chemical method that thermal decomposition and electronation are representative, can obtain narrow size distribution, Monodisperse nanocrystals product that pattern is unified, be synthesizing mean the most general at present.But the presoma that the raw material of chemical method is normally poisonous, and be difficult to remove, easily cause the problems such as product thing is mutually impure, accessory substance is toxic, see AdamsLLA, SweeneyWR, JaegerHM.GrowthofCadmiumNanocrystals [J] .TheJournalofPhysicalChemistryC, 2010,114 (14): 6304-6310.Laser method, as a kind of novel physics synthesis technique, is subject to people's attention in recent years gradually.When the method is for the synthesis of metal nanoparticle, overcome the defect of chemical method, there is the advantages such as thing is mutually pure, nontoxic, technique is simple simultaneously, reaction time is short, is the green safety synthesizing mean under normal temperature, see SemaltianosNG.Nanoparticlesbylaserablation [J] .CriticalReviewsinSolidStateandMaterialsSciences, 2010,35 (2): 105-124.But laser method is still to synthesize gold at present, the noble metal nano particles such as silver are main, see ZengH, DuXW, SinghSC, etal.Nanomaterialsvialaserablation/irradiationinliquid:a review [J] .AdvancedFunctionalMaterials, 2012, 22 (7): 1333-1353, the research prepared for active metal nano particle is also few, and Product size distribution very large (being usually greater than 15%), do not reach the application requirement of size uniform, the regulation and control to particle size are not realized yet, see HaiboZeng, WeipingCai, YueLi, JinlianHu, andPeishengLiu.Composition/StructuralEvolutionandOptical PropertiesofZnO/ZnNanoparticlesbyLaserAblationinLiquidMe dia [J] .2005, 109 (39), 18260-18266.
Summary of the invention
Object of the present invention, for the more difficult synthesis of existing preparation technology monodispersed active metal nano particle and cannot realize to active metal nanoparticle size regulation and control problem, utilize the quick green syt of laser ablation process and parallel laser irradiation technique can the feature of homogenising regulation and control size, a kind of method utilizing nanosecond laser ablation and the active nano particle of parallel laser irradiation controlledly synthesis single dispersing is in the liquid phase provided.
The present invention is achieved by following technical solution.
Utilize the method for laser controlledly synthesis single dispersing active metal nano particle, there are following steps:
(1) take pure metal targets as raw material, by target material surface sand papering to remove its oxide layer; Metal targets is placed in distilled water ultrasonic cleaning 2min, then is placed in cyclohexane ultrasonic cleaning 2min; In triplicate, natural air drying makes target material surface dry;
(2) in laser irradiating device, pass into argon gas, in the target embedding device that step (1) is handled well, add cyclohexane, and add oleic acid, make 0.05% < oleic acid volume solubility < 0.12%; Adopt ns focused pulse laser ablation target, the ablation time is 20min, obtained simple metal nano-sized colloidal solution;
(3) shift colloidal solution obtained in 8ml step (2) in another laser irradiating device, the oleic acid volumetric concentration in adjustable ring hexane is 0.14% ~ 0.17%; Stir and argon shield condition under, adopt nanosecond parallel pulse laser irradiation is carried out to simple metal nano-sized colloidal solution, exposure time is 20min, acquisition 5 ~ 20nm single dispersing active metal nano particle;
The metal targets of described step (1) is cadmium, zinc, iron, cobalt, nickel and other active metal, and target purity is 99.999%, and its thickness is 3 ~ 5mm.
The laser energy of the ns focused pulse laser ablation target of described step (2) is 60mJ, and laser repetition rate is 5Hz; The height of liquid medium and the distance between target upper surface and liquid level are 5mm.
Described step (3) nanosecond parallel veins impulse actinometric solutions laser energy be 200 ~ 350mJ, laser repetition rate is 10Hz; The height of liquid medium is 60 ~ 80mm.
Described step (3) changes laser energy density to realize the regulation and control to particle size by regulation voltage.
Add in described step (2) or (3) and stir magneton and stir, speed is 540r/min.
Described single dispersing active metal nano particle is the active metal nano particle of Size Distribution degree < 10%.
Instant invention overcomes existing preparation technology more difficult synthesis single dispersing active metal nano particle and the problem to the regulation and control of active metal nanoparticle size cannot be realized, in liquid phase at normal temperatures and pressures, achieving that pattern is unified, good dispersion and the controlledly synthesis of the active nano particle of Size Distribution degree < 10%.In addition, synthetic method craft of the present invention is simple, easy to operate, be easy to control, no coupling product and impurity, belongs to normal temperature and pressure and eco-friendly green synthesis process.The method is a kind of universality method, can be used for synthesizing most of active metals nano particle.
Accompanying drawing explanation
Fig. 1 be the present invention utilize nanosecond laser focusing ablating technics with the process flow diagram of parallel laser irradiation process unit synthesis single dispersing active metal nano particle;
Fig. 2 is the thing phase phenogram of cadmium nano particle in embodiment 1;
Fig. 3 is transmission electron microscope figure, the high power transmission electron microscope figure of cadmium nano particle in embodiment 1 and the particle diameter statistical chart to particle size;
Fig. 4 is transmission electron microscope figure, the high power transmission electron microscope figure of cadmium nano particle in embodiment 2 and the particle diameter statistical chart to particle size;
Fig. 5 is transmission electron microscope figure, the high power transmission electron microscope figure of cadmium nano particle in embodiment 3 and the particle diameter statistical chart to particle size;
Fig. 6 is transmission electron microscope figure, the high power transmission electron microscope figure of cadmium nano particle in embodiment 4 and the particle diameter statistical chart to particle size;
Fig. 7 is the transmission electron microscope figure of zinc nanoparticles in embodiment 5 and the particle diameter statistical chart to particle size.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
(1) with purity be 99.999%, the cadmium target of thickness 5mm for raw material, by target material surface sand papering to remove its oxide layer; Metal targets is placed in distilled water ultrasonic cleaning 2min, then is placed in cyclohexane ultrasonic cleaning 2min; In triplicate, natural air drying makes target material surface dry.
(2) as shown in Fig. 1 (a), cadmium target is placed in the oleic acid ethanolic solution of 20mL, oleic acid percent by volume is 0.1%, liquid level and cadmium target upper surface distance are 5mm, employing wavelength is that the ps pulsed laser and ns pulsed laser of 1064nm focuses on target upper surface, and laser energy density is about 120mJ/cm
2, repetition rate 5Hz; Whole process employing flow velocity is that the argon gas stream of 60sccm is protected, and prevents cadmium to be oxidized, and plays the effect getting rid of oxygen; And need stirring be aided with, add stirring magneton, mixing speed is 540r/min; The height of liquid medium and the distance between target upper surface and liquid level are 5mm; Namely abundant cadmium nano-sized colloidal solution is obtained after laser action 20min.
(3) 8ml solution is shifted in another laser irradiating device, as shown in Fig. 1 (b), oleic acid volumetric concentration in adjustable ring hexane is 0.15%, use parallel laser instead and carry out irradiation, adopt the argon gas flow velocity the same with step (2) and mixing speed, laser energy is 200mJ, and laser repetition rate is 10Hz; The height of liquid medium is 70mm, and irradiation 20min can obtain monodispersed cadmium nano particle.
As shown in Fig. 2 (a), by measurement and the Fast Fourier Transform (FFT) figure of high power transmission electron microscope figure and respective two-dimensional interplanar distance, can determine that particle is the cadmium of six side's phases mutually, the SEAD figure shown in Fig. 2 (b) further illustrates product and is six pure side's phase cadmium simple substance.
(a) ~ (c) of Fig. 3 is respectively transmission electron microscope figure, high power transmission electron microscope figure and the particle diameter statistical chart to particle size, can see that obtained particle dispersion is good from Fig. 3 (a), size uniform, Fig. 3 (b) then embodies the good crystallinity of individual particle, it is 16.9 ± 1.1nm that Fig. 3 (c) adds up by particle diameter the Product size that parallel pulse laser irradiation under known 200mJ energy obtains, Size Distribution degree 6.5%, reaches the requirement that single dispersing Size Distribution degree is less than 10%.To sum up, we obtain monodispersed cadmium nano particle by laser ablation process and parallel irradiation technique.
It should be noted that it is all necessary for stirring in these (2), (3) two steps, stir the nanocrystalline laser action region that speeds away that can make generation in the first step, avoid the secondary action of laser; Stir the nanocrystalline irradiation evenly receiving parallel laser fully made in solution in second step, be convenient to the product obtaining size uniform, save exposure time simultaneously, raise the efficiency.
In addition, in these (2), (3) two steps, oleic acid concentration has a significant impact the formation of product and uniformity.Such as, it is coated that the nano grain surface obtained during non-refuelling acid has carbon-coating; When oleic acid concentration is 0.5%, nanoparticle size uniformity declines to a great extent; When oleic acid concentration is 1%, the corrasion due to acid makes product be nanometer fragment, disorderly and unsystematic.
Embodiment 2
Relative to embodiment 1, in step (3), laser energy parameter changes 250mJ into, and all the other conditions are constant, and the corresponding sign of single dispersing cadmium nano particle obtained is as shown in Fig. 4 (a) ~ (c).Can see that obtained particle dispersion is good from Fig. 4 (a), size uniform, Fig. 4 (b) then embodies the good crystallinity of individual particle, it is 13.6 ± 1.0nm that Fig. 4 (c) adds up by particle diameter the Product size that parallel pulse laser irradiation under known 250mJ energy obtains, Size Distribution degree 7.3%, has equally also arrived the requirement that single dispersing Size Distribution degree is less than 10%.
Embodiment 3
Relative to embodiment 1, in step (3), laser energy parameter changes 300mJ into, all the other conditions are constant, the corresponding sign of single dispersing cadmium nano particle obtained is as shown in Fig. 5 (a) ~ (c), can see that obtained particle dispersion is good from Fig. 5 (a), size uniform, Fig. 5 (b) then embodies the good crystallinity of individual particle, it is 10.1 ± 1.0nm that Fig. 5 (c) adds up by particle diameter the Product size that parallel pulse laser irradiation under known 300mJ energy obtains, Size Distribution degree 9.9%, equally also arrive the requirement that single dispersing Size Distribution degree is less than 10%.
Embodiment 4
Relative to embodiment 1, in step (3), laser energy parameter changes 350mJ into, all the other conditions are constant, the corresponding sign of single dispersing cadmium nano particle obtained is as shown in Fig. 6 (a) ~ (c), can see that obtained particle dispersion is good from Fig. 6 (a), size uniform, Fig. 6 (b) then embodies the good crystallinity of individual particle, it is 6.5 ± 0.8nm that Fig. 6 (c) adds up by particle diameter the Product size that parallel pulse laser irradiation under known 350mJ energy obtains, Size Distribution degree 12.3%, close to the requirement that single dispersing Size Distribution degree is less than 10%.
In addition, by the longitudinal direction contrast of individual particle in Fig. 3 (b), Fig. 4 (b), Fig. 5 (b), Fig. 6 (b), can see the rising along with laser energy during irradiation, particle mean size is reduction trend.
Embodiment 5
Relative to embodiment 1, by the zinc target that the target raw material in step (1) replaces with purity 99.999%, thickness is 5mm, other condition is identical with embodiment 1, the obtained corresponding sign of zinc nanoparticles as shown in Figure 7, can see that particle dispersion is good from Fig. 7 (a), size uniform, it is 14.1 ± 1.0nm that Fig. 7 (b) adds up by particle diameter the Product size that parallel pulse laser irradiation under known 200mJ energy obtains, Size Distribution degree 7.1%, reaches the requirement that single dispersing Size Distribution degree is less than 10%.Namely monodispersed zinc nanoparticles is obtained by laser ablation process with parallel irradiation technique.Equally, if target raw material is replaced with iron, cobalt, nickel and other active metals, also can obtain corresponding single dispersing active metal nano particle completely, seldom repeat at this.
Claims (7)
1. utilize a method for laser controlledly synthesis single dispersing active metal nano particle, there are following steps:
(1) take pure metal targets as raw material, by target material surface sand papering to remove its oxide layer; Metal targets is placed in distilled water ultrasonic cleaning 2min, then is placed in cyclohexane ultrasonic cleaning 2min; In triplicate, natural air drying makes target material surface dry;
(2) in laser irradiating device, pass into argon gas, in the target embedding device that step (1) is handled well, add cyclohexane, and add oleic acid, make 0.05% < oleic acid volume solubility < 0.12%; Adopt ns focused pulse laser ablation target, the ablation time is 20min, obtained simple metal nano-sized colloidal solution;
(3) shift colloidal solution obtained in 8ml step (2) in another laser irradiating device, the oleic acid volumetric concentration in adjustable ring hexane is 0.14% ~ 0.17%; Stir and argon shield condition under, adopt nanosecond parallel pulse laser irradiation is carried out to simple metal nano-sized colloidal solution, exposure time is 20min, acquisition 5 ~ 20nm single dispersing active metal nano particle.
2. the method utilizing laser controlledly synthesis single dispersing active metal nano particle according to claim 1, it is characterized in that, the metal targets of described step (1) is cadmium, zinc, iron, cobalt, nickel and other active metal, and target purity is 99.999%, and its thickness is 3 ~ 5mm.
3. the method utilizing laser controlledly synthesis single dispersing active metal nano particle according to claim 1, is characterized in that, the laser energy of the ns focused pulse laser ablation target of described step (2) is 60mJ, and laser repetition rate is 5Hz; The height of liquid medium and the distance between target upper surface and liquid level are 5mm.
4. the method utilizing laser controlledly synthesis single dispersing active metal nano particle according to claim 1, it is characterized in that, described step (3) nanosecond parallel veins impulse actinometric solutions laser energy be 200 ~ 350mJ, laser repetition rate is 10Hz; The height of liquid medium is 60 ~ 80mm.
5. the method utilizing laser controlledly synthesis single dispersing active metal nano particle according to claim 1, is characterized in that, described step (3) changes laser energy density to realize the regulation and control to particle size by regulation voltage.
6. the method utilizing laser controlledly synthesis single dispersing active metal nano particle according to claim 1, is characterized in that, adds to stir magneton and stir in described step (2) or (3), and speed is 540r/min.
7. the method utilizing laser controlledly synthesis single dispersing active metal nano particle according to claim 1, is characterized in that, described single dispersing active metal nano particle is the active metal nano particle of Size Distribution degree < 10%.
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| CN102717083B (en) * | 2012-05-28 | 2014-07-09 | 天津大学 | Method for preparing cadmium metal nano particles by laser |
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| CN103508451A (en) * | 2013-10-09 | 2014-01-15 | 江苏大学 | Method and device for nanosecond pulse laser-assisted preparation of nano-diamond |
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