CN104014800A - Preparing method for controllably synthesizing monodisperse active metal nanoparticles through lasers - Google Patents
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Abstract
The invention discloses a preparing method for controllably synthesizing monodisperse active metal nanoparticles through lasers. The method comprises the steps that pure-metal target materials serve as raw materials, the processed target materials are placed into a laser radiating device, the laser radiating device is inflated with argon, cyclohexane and oleic acid are added into the laser radiating device, and then the volume solubility of the oleic acid is larger than 0.05 percent but smaller than 0.12 percent; the target materials are ablated through a nanosecond focus pulse laser to prepare a pure-metal nanometer colloid solution; the colloid solution is transferred to the other laser radiating device, and the volume concentration of the oleic acid in the cyclohexane is adjusted to range from 0.14 percent to 0.17 percent; a nanosecond parallel pulse laser is utilized for irradiating the metal nanometer colloid solution to prepare the monodisperse active metal nanoparticles with the diameter ranging from 5 nm to 20 nm. According to the preparing method, the active metal nanoparticles uniformed in appearance under the normal-temperature and normal-pressure liquid phase condition are controllably synthesized, and the size distribution of the active nanometer particles is smaller than 10 percent. The method is simple in technology, convenient to operate, free of by-products and impurities and suitable for synthesizing most active metal nanometer particles, and is an environmental-friendly synthesizing technology.
Description
Technical field
The present invention the invention relates to metal nanoparticle, the preparation method that particularly the controlled laser method of a kind of size synthesizes monodispersed active metal nano particle.
Background technology
Active metal nano particle possesses the peculiar skin effect of 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.For example, 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, referring to Pankhurst Q A, Connolly J, Jones S K, et al.Applications of magnetic nanoparticles in biomedicine[J] .Journal of physics D:Applied physics, 2003,36 (13): R167.Simultaneously, the physicochemical properties such as optical, electrical, the magnetic of nano particle and its size and pattern are closely bound up, very responsive to change in size, can be along with the change generation marked change of grain diameter, referring to Puntes V F, Krishnan K M, Alivisatos A P.Colloidal nanocrystal shape and size control:the case of cobalt[J] .Science, 2001,291 (5511): 2115-2117.Therefore the active metal nano particle that, preparation is single to be disperseed (being that pattern is unified, good dispersion, distribution of sizes degree < 10%) is also realized the regulation and control of its size is had to meaning.
Due to the existence of the problems such as activity is high, oxidizable, easy reunion, synthetic 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 as the chemical method of representative taking thermal decomposition and electronation, can obtain narrow size distribution, Monodisperse nanocrystals product that pattern is unified, be the most general synthesizing mean 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, referring to Adams L L A, Sweeney W R, Jaeger H M.Growth of Cadmium Nanocrystals[J] .The Journal of Physical Chemistry C, 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.The method is during 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, referring to Semaltianos N G.Nanoparticles by laser ablation[J] .Critical Reviews in Solid State and Materials Sciences, 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, referring to Zeng H, Du X W, Singh S C, et al.Nanomaterials via laser ablation/irradiation in liquid:a review[J] .Advanced Functional Materials, 2012, 22 (7): 1333-1353, the research of preparing for active metal nano particle is also few, and product distribution of sizes is large (being greater than 15%) conventionally very, do not reach the application requirements of size uniform, do not realize the regulation and control to particle size yet, referring to Haibo Zeng, Weiping Cai, Yue Li, Jinlian Hu, and Peisheng Liu.Composition/Structural Evolution and Optical Properties of ZnO/Zn Nanoparticles by Laser Ablation in Liquid Media[J] .2005, 109 (39), 18260-18266.
Summary of the invention
Object of the present invention, synthesize monodispersed active metal nano particle and cannot realize the problem to the regulation and control of active metal nanoparticle size for existing preparation technology is more difficult, utilize the laser ablation process feature that fast green synthetic and parallel laser irradiation technique can homogenising regulation and control size, a kind of method of utilizing nanosecond laser ablation to disperse active nano particle with parallel laser irradiation controlledly synthesis list in liquid phase is provided.
The present invention is achieved by following technical solution.
Utilize laser controlledly synthesis list to disperse the method for active metal nano particle, there are following steps:
(1) taking pure metal targets as raw material, by target material surface with sand papering to remove its oxide layer; Metal targets is placed in to 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 nanosecond focusing pulse laser ablation target, the ablation time is 20min, makes simple metal nano-sized colloidal solution;
(3) shift the colloidal solution making in 8ml step (2) to another laser irradiating device, the oleic acid volumetric concentration in adjustable ring hexane is 0.14%～0.17%; Under the condition of stirring and argon shield, employing nanosecond, parallel pulse laser carried out irradiation to simple metal nano-sized colloidal solution, and exposure time is 20min, obtained single active metal nano particle that disperses of 5～20nm.
The metal targets of described step (1) is cadmium, zinc, iron, cobalt, nickel and other active metal, and target purity is 99.999%, and target thickness is 3～5mm.
Described step (2) nanosecond focusing pulse laser ablation target laser energy be 60mJ, laser repetition rate is 5Hz; The height of liquid medium is that the distance between target upper surface and liquid level is 5mm.
Described step (3) nanosecond parallel pulse laser irradiating soln 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.
In described step (2) or (3), all add stirring magneton to stir, speed is 540r/min.
Described single dispersion active metal nano particle is the active metal nano particle of distribution of sizes degree < 10%.
The present invention has overcome the more difficult synthetic single dispersion active metal nano particle of existing preparation technology and cannot realize the problem to the regulation and control of active metal nanoparticle size, has realized the controlledly synthesis of the active nano particle of pattern unification, good dispersion and distribution of sizes degree < 10% in liquid phase at normal temperatures and pressures.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.
Brief description of the drawings
Fig. 1 is that the present invention utilizes nanosecond laser focusing ablating technics and the synthetic single process flow diagram that disperses active metal nano particle of parallel laser irradiation process unit;
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) taking purity as 99.999%, the cadmium target of thickness 5mm is as raw material, by target material surface with sand papering to remove its oxide layer; Metal targets is placed in to 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 to 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, adopt the ps pulsed laser and ns pulsed laser that wavelength is 1064nm to focus on target upper surface, laser energy density is about 120mJ/cm
2, repetition rate 5Hz; Whole process adopts the argon gas stream that flow velocity is 60sccm to protect, and prevents that cadmium is oxidized, and plays the effect of getting rid of oxygen; And need be aided with stirring, and adding stirring magneton, mixing speed is 540r/min; The height of liquid medium is that the distance between target upper surface and liquid level is 5mm; After laser action 20min, obtain abundant cadmium nano-sized colloidal solution.
(3) shift 8ml solution to 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 argon gas flow velocity and the mixing speed the same with step (2), 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.
Fig. 3 (a)～(c) is respectively transmission electron microscope figure, high power transmission electron microscope figure and the particle diameter statistical chart to particle size, can see that from Fig. 3 (a) particle dispersion making is good, size uniform, Fig. 3 (b) has embodied the good crystallinity of individual particle, Fig. 3 (c) adds up by particle diameter the product that under known 200mJ energy, parallel pulse laser irradiation obtains and is of a size of 16.9 ± 1.1nm, distribution of sizes degree 6.5%, reaches the requirement that single dispersion size degree of distribution is less than 10%.To sum up, we have obtained monodispersed cadmium nano particle by laser ablation process and parallel irradiation technique.
It should be noted that it is all necessary in these (2), (3) two steps, stirring, in the first step, stir the nanocrystalline laser action region that speeds away that can make generation, avoid the secondary action of laser; In second step, stir the nanocrystalline irradiation of evenly receiving fully parallel laser making in solution, be convenient to obtain the product of size uniform, save exposure time simultaneously, raise the efficiency.
In addition, in these (2), (3) two steps, formation and the uniformity of oleic acid concentration to product has a significant impact.It is coated that the nano grain surface for example, obtaining when, non-refuelling is sour has carbon-coating; In the time that oleic acid concentration is 0.5%, nanoparticle size uniformity declines to a great extent; In the time that oleic acid concentration is 1%, because making product, sour corrasion is nanometer fragment, disorderly and unsystematic.
Embodiment 2
With respect to embodiment 1, laser energy parameter changes 250mJ in step (3), and all the other conditions are constant, and the single corresponding sign of cadmium nano particle of disperseing obtaining is as shown in Fig. 4 (a)～(c).Can see that from Fig. 4 (a) particle dispersion making is good, size uniform, Fig. 4 (b) has embodied the good crystallinity of individual particle, Fig. 4 (c) adds up by particle diameter the product that under known 250mJ energy, parallel pulse laser irradiation obtains and is of a size of 13.6 ± 1.0nm, distribution of sizes degree 7.3%, equally also to the requirement that is less than 10% of single dispersion size degree of distribution.
Embodiment 3
With respect to embodiment 1, in step (3), laser energy parameter changes 300mJ into, all the other conditions are constant, the single corresponding sign of cadmium nano particle of disperseing obtaining is as shown in Fig. 5 (a)～(c), can see that from Fig. 5 (a) particle dispersion making is good, size uniform, Fig. 5 (b) has embodied the good crystallinity of individual particle, Fig. 5 (c) adds up by particle diameter the product that under known 300mJ energy, parallel pulse laser irradiation obtains and is of a size of 10.1 ± 1.0nm, distribution of sizes degree 9.9%, equally also to the requirement that is less than 10% of single dispersion size degree of distribution.
Embodiment 4
With respect to embodiment 1, in step (3), laser energy parameter changes 350mJ into, all the other conditions are constant, the single corresponding sign of cadmium nano particle of disperseing obtaining is as shown in Fig. 6 (a)～(c), can see that from Fig. 6 (a) particle dispersion making is good, size uniform, Fig. 6 (b) has embodied the good crystallinity of individual particle, Fig. 6 (c) adds up by particle diameter the product that under known 350mJ energy, parallel pulse laser irradiation obtains and is of a size of 6.5 ± 0.8nm, distribution of sizes degree 12.3%, approaches the requirement that single dispersion size degree of distribution is less than 10%.
In addition, by longitudinal contrast of individual particle in Fig. 3 (b), Fig. 4 (b), Fig. 5 (b), Fig. 6 (b), the rising of laser energy can see along with irradiation time, particle mean size is and reduces trend.
Embodiment 5
With respect to embodiment 1, target raw material in step (1) is replaced with to the zinc target that purity 99.999%, thickness are 5mm, other condition is identical with embodiment 1, the corresponding sign of zinc nanoparticles making as shown in Figure 7, can see that from Fig. 7 (a) particle dispersion is good, size uniform, Fig. 7 (b) adds up by particle diameter the product that under known 200mJ energy, parallel pulse laser irradiation obtains and is of a size of 14.1 ± 1.0nm, distribution of sizes degree 7.1%, has reached the requirement that single dispersion size degree of distribution is less than 10%.Obtained monodispersed zinc nanoparticles by laser ablation process with parallel irradiation technique.Equally, if target raw material is replaced with to iron, cobalt, nickel and other active metals, also can obtain corresponding single active metal nano particle that disperses completely, seldom repeat at this.
Claims (7)
1. utilize laser controlledly synthesis list to disperse a method for active metal nano particle, there are following steps:
(1) taking pure metal targets as raw material, by target material surface with sand papering to remove its oxide layer; Metal targets is placed in to 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 nanosecond focusing pulse laser ablation target, the ablation time is 20min, makes simple metal nano-sized colloidal solution;
(3) shift the colloidal solution making in 8ml step (2) to another laser irradiating device, the oleic acid volumetric concentration in adjustable ring hexane is 0.14%～0.17%; Under the condition of stirring and argon shield, employing nanosecond, parallel pulse laser carried out irradiation to simple metal nano-sized colloidal solution, and exposure time is 20min, obtained single active metal nano particle that disperses of 5～20nm.
2. the method for utilizing laser controlledly synthesis list to disperse 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 target thickness is 3～5mm.
3. the method for utilizing laser controlledly synthesis list to disperse active metal nano particle according to claim 1, is characterized in that, described step (2) nanosecond focusing pulse laser ablation target laser energy be 60mJ, laser repetition rate is 5Hz; The height of liquid medium is that the distance between target upper surface and liquid level is 5mm.
4. the method for utilizing laser controlledly synthesis list to disperse active metal nano particle according to claim 1, it is characterized in that, described step (3) nanosecond parallel pulse laser irradiating soln laser energy be 200～350mJ, laser repetition rate is 10Hz; The height of liquid medium is 60～80mm.
5. the method for utilizing laser controlledly synthesis list to disperse 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 for utilizing laser controlledly synthesis list to disperse active metal nano particle according to claim 1, is characterized in that, all adds stirring magneton to stir in described step (2) or (3), and speed is 540r/min.
7. the method for utilizing laser controlledly synthesis list to disperse active metal nano particle according to claim 1, is characterized in that, described single dispersion active metal nano particle is the active metal nano particle of distribution of sizes degree < 10%.
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