CN101774023A - Preparation method of monodispersed-precious metal nanoparticles in liquid phase by using pulse laser ablation - Google Patents
Preparation method of monodispersed-precious metal nanoparticles in liquid phase by using pulse laser ablation Download PDFInfo
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Abstract
The present invention discloses a preparation method of monodispersed-precious metal nanoparticles in liquid phase by using pulse laser ablation, comprising the following steps: putting a precious metal target and a metal target in a container filled with liquid phase material, placing the container in an ultrasonic dispersion tank, making the ultrasonic dispersion tank work at an oscillation frequency between 60 to 85 Hz; focusing the beam of pulse laser on the contact surface of the precious metal and the liquid phase material to generate the plasma plume, performing the ablation deposition reaction for 20 to 40 minutes, adjusting the laser beam to make the beam focus on the contact surface of the metal and the liquid phase material, performing the ablation deposition reaction for 20 to 40 minutes, and stopping the irradiate of the pulse laser beam; taking out the reacted liquid phase material, drying and separating to obtain the monodispersed-precious metal nanoparticles. The invention has the advantages of simple operation, low cost, good dispersibility, non-pollution and non-toxic and can be directly used in biosystem.
Description
Technical field
The invention belongs to the preparation field of noble metal nano particles, particularly a kind of method of in liquid phase environment, carrying out the noble metal nano particles of pulse laser ablation prepared in reaction monodisperse sphere shape.
Background technology
Noble metal nano particles has special physical property, and they are widely used in fields such as catalysis, biomarker, photoelectronics, information storage and SERS.To the research of noble metal nano particles, be the forward position focus of material science and association area especially to the controlled preparation of its pattern and corresponding character thereof and application study always.In recent years, obtaining significant progress aspect the gold nano-material research, people prepare the gold nano grain of multiple pattern, and it is widely used in fields such as nano-device structure, biomarker, medical science detection and information storage.
Up to the present, had the synthetic method of many kinds of noble metal nano particles to be studied and to have developed, main method has chemical reduction method, photodissociation method, pyrolysismethod, ultrasonic wave decomposition method, electrolysis etc.For example; people can be by adopting different protective agents (alkyl hydrosulfide, water-soluble polymer and long-chain amine etc.), different noble metal precursor body and reducing agent, and different reducing environments; synthetic as gas phase, the synthetic single noble metal nano particles that disperses of preparation that waits of liquid phase.Wherein, the application of liquid phase synthetic technology is the most widely, and its synthetic method is also comparatively ripe, can control and finishing the size of noble metal nano particles.
Because noble metal nano particles has good electricity, optics, magnetic property, they are applied to catalysis, electronics, biologic applications and clinical diagnosis etc. widely; And noble metal nano particles is necessary in a lot of its dispersivenesses of Application for Field, as the Size Distribution standard variance less than 5% monodisperse hydrophobic metal nanoparticle under entropy drives, can form flawless large-area ordered array; And the two-dimensional array that obtains by the polydispersion gold nano grain, the degree of order is poor, defective is many, makes the prerequisite that the orderly zero defect array of large-area two-dimensional is considered to nano electron device.Height mono-dispersed nano particle can also be used to construct the three-dimensional order assembly, and the three-dimensional order assembly is potential photonic crystal, can be used for controlling the propagation of light.On the other hand, metal nanoparticle is easy to oxidized and is easy to reunite, thereby makes metal nanoparticle can lose a part of special nature.Therefore, a lot of research work are devoted to protect the dispersiveness of noble metal nano particles.
The pulse laser ablation reaction is as a kind of technology that is used to prepare nano material and nanostructured preparation in the liquid phase, and it has characteristics such as controlled within the specific limits, that reaction atmosphere impurity content is few.Its cardinal principle is the solid reaction target surface of pulse laser focusing in liquid, makes reaction target surface produce high temperature and fusion, thereby produce the plasma plume brightness in liquid-solid interface; The restriction that the plasma plume brightness can be subjected to liquid produces a HTHP district, and this zone is the necessary condition that provides of some chemical reactions, as the reaction between the reaction between the ablation thing, ablation thing and the liquid etc.; Along with the end of a pulsed laser energy, the plasma plume cooling, thus in liquid, form little-Na particle.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art part, primary and foremost purpose of the present invention is to provide a kind of quick single method of disperseing noble metal nano particles for preparing.
Another purpose of the present invention is to provide a kind of single noble metal nano particles that disperses of method for preparing; This grain diameter is little, narrowly distributing, the noble metal nano particles of monodispersity.
A further object of the present invention is to provide above-mentioned single noble metal nano particles that disperses in biology, optics, catalysis, and Application for Field such as medical science.
Purpose of the present invention realizes by following technical scheme: a kind ofly utilize pulse laser to ablate in liquid phase environment prepare the singly method of dispersion noble metal nano particles, comprise the steps:
Noble metal target and metal targets are put into the container that liquid phase substance is housed, and container is placed in the ultrasonic dispersion slot, make of the frequency of oscillation work (the ablation product of back formation after rapidly scattered, help the dispersion of gold nano grain) of ultrasonic dispersion slot with 60～85kHz; Pulsed laser beam is focused on the contact surface of noble metal target and liquid phase substance, contact surface produces plasma plume, after the ablation deposition reaction is carried out 20～40 minutes, regulate laser beam, make laser beam focus on the contact surface of metal targets and liquid phase substance, after the reaction of ablating is carried out 20～40 minutes, the stop pulse laser beam irradiation; Reacted liquid phase substance is taken out, and drying is separated, and obtains single noble metal nano particles that disperses.
Described noble metal target is gold, silver or platinum, is high-purity target (purity is mass content 99%～99.99%); The target thickness of described noble metal target is 3～5 millimeters, is shaped as circular or square; The surface of described noble metal target polishes processing.
Described metal targets is aluminium, magnesium or zinc, is high-purity target (purity is mass content 99%～99.99%); The thickness of described metal targets is 3～5 millimeters, is shaped as circular or square; The surface of described metal targets polishes processing.
Described container is quartz container or glass container.
Described focusing is that pulsed laser beam is focused on by condenser lens; The upper surface of described liquid phase substance exceeds noble metal target or metal targets upper surface 3～10mm.
Described liquid phase substance is a deionized water.
Described drying is vacuum drying, and dry temperature is 60～120 ℃.
A kind of single noble metal nano particles that disperses by method for preparing.The particle diameter of described single dispersion noble metal nano particles is 5～30nm.
Above-mentioned single noble metal nano particles that disperses can be applicable to fields such as nano-device structure, biomarker, medical science detection and information storage.For example monodispersed gold nano grain can be used to construct the three-dimensional order assembly, and the three-dimensional order assembly is potential photonic crystal, can be used for controlling the propagation of light; And for example the gold nano grain of employing protein labeling such as thanh has developed a kind of immune agglutination analytic approach of highly sensitive detection albumin A antibody; In addition, single disperse gold nano grain can also be used to verify basic theories and as the standard substance that rectifies an instrument etc., therefore singly disperse the preparation of noble metal nano particles very meaningful.
Principle of the present invention is: the present invention is placed on noble metal and metal reaction target in the liquid phase substance simultaneously, at first make pulsed laser beam focus on the noble metal target material upper surface, utilize the high-energy of pulse laser, make the surface mass fusion of noble metal target material also and then at the target upper surface form plasma plume by laser ablation, the restriction that the plasma plume brightness can be subjected to liquid produces a HTHP district, the necessary condition that provides of some chemical reactions is provided in this zone, as the reaction between the reaction between the ablation thing, ablation thing and the liquid etc.; The plasma plume brightness is (the process required time is in nanosecond or microsecond magnitude) cancellation at a terrific speed; After laser pulse finished, the material that is in molten state during beginning can condense because of cooling and generate noble metal nano particles.Because the noble metal nano particles surface has the electric charge of uneven distribution, and has very big specific surface energy, is easy to reunite in liquid; Form unsettled noble metal nano colloid.Regulating impulse laser beam and focus on metal reaction target upper surface then, reaction can make metal oxide by ablating; And noble metal nano particles can adsorb metal oxide in the surface, thereby can shield the electrostatic effect between noble metal nano particles, makes the above-mentioned noble metal nano particles that makes have good monodispersity.
The present invention compared with prior art has following advantage and beneficial effect:
(1) the present invention utilizes the pulse laser ablation technology to make the noble metal nano particles of monodispersity first in liquid phase substance, this method is simple to operate, with low cost, and do not have harsh operating environment requirement, can under normal temperature and pressure conditions, realize the preparation of product.
(2) single preparation method who disperses noble metal nano particles provided by the invention, it is the pulse laser ablation technology of in the high purity water environment, utilizing, compare with traditional chemical synthesising technology with ablation noble metal target material technology in the present simple laser liquid, has good dispersion, pollution-free, nontoxic, can directly apply to beneficial effects such as living things system.
Description of drawings
Fig. 1 uses the structural representation of equipment for the present invention.
Fig. 2 is the field emission electromicroscopic photograph figure that embodiment 1 gained list disperses gold nano grain.
Fig. 3 is transmission electron microscope photo and the size statistical chart that embodiment 1 gained list disperses gold nano grain, and wherein (a) is transmission electron microscope photo figure, (b) is the high-resolution photo figure of a gold nano grain; (c) be the size distribution plot of gold nano grain under the transmission electron microscope.
Fig. 4 is the uv-visible absorption spectra figure that embodiment 1 gained list disperses gold nano grain.
The specific embodiment
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing, but embodiments of the present invention are not limited thereto.
Embodiment 1:
As shown in Figure 1, equipment of the present invention has comprised that laser instrument 1 (adopts the Nd:YAG pulse laser, optical maser wavelength 532nm, pulsewidth 10ns, energy is 2.95mJ, and frequency is 5Hz or 10Hz), completely reflecting mirror 2, condenser lens 3 (its focal length is 300mm), quartz container 4, noble metal reaction target 5, metal reaction target 6, ultrasonic dispersion slot 7.
As shown in Figure 2, for single field emission microscope photo that disperses gold nano grain that present embodiment is prepared, see that from figure the particle diameter of gold nano grain is 200～500nm, the surface is smoother all.
(b) shown in (c), be respectively single transmission electron microscope photo that disperses gold nano grain of present embodiment preparation as Fig. 3 (a), the high-resolution photo of a gold nano grain, and the size distribution plot of gold nano grain under the transmission electron microscope.By analyzing as can be known, it is 14nm that this list disperses the average grain diameter of gold nano grain, has the structure of cubic system.
As shown in Figure 4, the uv-visible absorption spectra that disperses gold nano grain for the list of present embodiment preparation.The absworption peak at 515nm place is the single plasma resonance absworption peak that disperse gold nano grain surface cause of particle diameter at 2～40nm among the figure.
Embodiment 2:
Adopt the used equipment of embodiment 1, high-purity gold reaction target (purity is 99.99%, thickness 3mm) and reactive magnesium target (purity is 99.99%, thickness 3mm) are put into glass container, then glass container is put into ultrasonic dispersion slot, make of the frequency of oscillation work of ultrasonic dispersion slot with 85kHz.In glass container, inject deionized water, make deionized water submergence gold reaction target, and make liquid level be higher than the upper surface 10mm of gold reaction target; Regulate laser optical path, the pulsed laser beam that makes the laser instrument emission focuses on the contact surface of gold reaction target and deionized water after by speculum and focus lamp, and laser frequency is 10Hz; After pulse laser ablation reaction is carried out 40 minutes, regulate laser beam, make pulsed laser beam focus on the contact surface of reactive magnesium target and deionized water by focus lamp, after 20 minutes, close laser instrument at pulse laser ablation reactive aluminum target.Reacted deionized water is taken out and it is dropped on the monocrystalline silicon piece substrate, put into vacuum drying chamber and carry out drying, be cooled to room temperature, the spherical gold nano grain product that can obtain disperseing with 60 ℃.Products obtained therefrom is carried out various tests (comprising field emission microscope, transmission electron microscope, X-ray diffraction).Take out reacted deionized water in addition and do the uv-visible absorption spectra test, can obtain an absworption peak at the 518nm place, the particle diameter that the spherical gold nano grain that disperses is described is at 2～40nm.
Embodiment 3:
Adopt the used equipment of embodiment 1, high-purity silver reaction target (purity is 99.99%, thickness 4mm) and zinc reaction target (purity is 99.99%, thickness 4mm) are put into quartz container, then quartz container is put into ultrasonic dispersion slot, make of the frequency of oscillation work of ultrasonic dispersion slot with 75kHz.In quartz container, inject deionized water, make deionized water submergence reaction target, and the upper surface 3mm that liquid level is higher than react target; Regulate laser optical path, the pulsed laser beam that makes the laser instrument emission focuses on the contact surface of silver reaction target and deionized water after by speculum and focus lamp, and laser frequency is 5Hz; After the pulse laser ablation reaction is carried out 20 minutes, regulate laser beam, make pulsed laser beam focus on the contact surface that zinc reacts target and deionized water by focus lamp, after 40 minutes, close laser instrument at pulse laser ablation aluminium target.Reacted deionized water is taken out and it is dropped on the monocrystalline silicon piece substrate, put into vacuum drying chamber and carry out drying.The monocrystalline silicon piece substrate is taken field emission microscope and transmission electron microscope is transferred big observation, can see and see on the substrate that the spherical silver of dispersion nano particle is arranged.Take out reacted deionized water in addition and do the uv-visible absorption spectra test, can obtain an absworption peak at the 410nm place, the particle diameter that the spherical silver nano particle that disperses is described is at 2～40nm.
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spiritual essence of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (9)
1. one kind is utilized pulse laser to ablate to prepare single method of disperseing noble metal nano particles in liquid phase environment, it is characterized in that comprising the steps:
Noble metal target and metal targets are put into the container that liquid phase substance is housed, and container is placed in the ultrasonic dispersion slot, make of the frequency of oscillation work of ultrasonic dispersion slot with 60～85kHz; Pulsed laser beam is focused on the contact surface of noble metal target and liquid phase substance, contact surface produces plasma plume, after the ablation deposition reaction is carried out 20～40 minutes, regulate laser beam, make laser beam focus on the contact surface of metal targets and liquid phase substance, after the reaction of ablating is carried out 20～40 minutes, the stop pulse laser beam irradiation; Reacted liquid phase substance is taken out, and drying is separated, and obtains single noble metal nano particles that disperses.
2. a kind of single method of disperseing noble metal nano particles of utilizing pulse laser in liquid phase environment, to ablate to prepare according to claim 1, it is characterized in that: described noble metal target is gold, silver or platinum; The target thickness of described noble metal target is 3～5 millimeters, is shaped as circular or square; The surface of described noble metal target polishes processing.
3. a kind of single method of disperseing noble metal nano particles of utilizing pulse laser in liquid phase environment, to ablate to prepare according to claim 1, it is characterized in that: described metal targets is aluminium, magnesium or zinc; The thickness of described metal targets is 3～5 millimeters, is shaped as circular or square; The surface of described metal targets polishes processing.
4. a kind of single method of disperseing noble metal nano particles of utilizing pulse laser in liquid phase environment, to ablate to prepare according to claim 1, it is characterized in that: described container is quartz container or glass container; The upper surface of described liquid phase substance exceeds noble metal target or metal targets upper surface 3～10mm.
5. a kind of single method of disperseing noble metal nano particles of utilizing pulse laser in liquid phase environment, to ablate to prepare according to claim 1, it is characterized in that: described focusing is that pulsed laser beam is focused on by condenser lens; The frequency of described laser beam is 5～10Hz.
6. a kind of single method of disperseing noble metal nano particles of utilizing pulse laser to ablate in liquid phase environment to prepare according to claim 1, it is characterized in that: described liquid phase substance is a deionized water.
7. a kind of single method of disperseing noble metal nano particles of utilizing pulse laser in liquid phase environment, to ablate to prepare according to claim 1, it is characterized in that: described drying is vacuum drying, dry temperature is 60～120 ℃.
8. the list by each described method preparation of claim 1～7 disperses noble metal nano particles.
9. single noble metal nano particles that disperses according to claim 8, it is characterized in that: the particle diameter of described single dispersion noble metal nano particles is 5～30nm.
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