CN104772465A - Noble metal nanostructure as well as preparation method and application thereof - Google Patents
Noble metal nanostructure as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a preparation method of a noble metal nanostructure. The preparation method comprises the following steps: putting a noble metal sheet in a solution containing nano graphene oxide, and carrying out ablation on the noble metal sheet by using pulse laser to obtain the noble metal nanostructure. The noble metal nanostructure prepared by using the preparation method is more uniform in size and appearance and controllable in grain size; with the increase of the concentration of a nano graphene oxide seed promoter, the size of a gold nanostructure becomes smaller and smaller and the dispersity becomes better and better; the prepared gold nanostructure system is pure, free of chemical residual and good in biocompatibility and lays a favorable foundation on the subsequent study in the biomedical field; the preparation method is simple and easily controllable in conditions.
Description
Technical field
The invention belongs to the preparation field of nano material, be specifically related to a kind of noble metal nano structure, Preparation Method And The Use, relating to a kind of further take nano graphene oxide as the preparation method of noble metal nano structure of the seed promoters mediation of seed promoters, noble metal nano structure prepared and uses thereof.
Background technology
Because nano material has small-size effect, skin effect, quantum effect, and the special nature such as the sound of nanostructured uniqueness, optical, electrical, thermal and magnetic, the design of nano material, assembling and application have become the study hotspot in the fields such as chemistry, material and biomedicine.
Noble metal nano structure is as a kind of important nano material, and its application can trace back to mid-term the 17th century, is often used by as pigment and medicine, as made ruby glass, chromatic ceramics etc.Along with the progress of science and technology, noble metal nano particles due to the physicochemical property of its uniqueness, the various fields such as extensive use biomarker, medical image, surface-enhanced Raman, photoelectronics.
Gold nano grain is as the Typical Representative of noble metal structures, and because it has good biocompatibility, the good characteristics such as high electron density have obtained and studied widely.The method of what current people commonly used prepare gold nano grain has following several: chemical reduction method, seeded growth method, two phase process, reverse microemulsion process, template, photochemical syntheses method etc.
Compare above chemical method and prepare gold nano grain, liquid-phase pulse laser ablation (PLA) technology is the technology that a kind of novel top-down prepares nano particle.Its principle is by a branch of high energy pulse laser, is irradiated to the metal targets in solution, makes its molting and gasifying, and after entering liquid phase, cooling forms nano particle.This method has that preparation method is simple, the cycle is short; Physics synthetic method, product system is pure, without other reagent that chemical reaction is brought into; The advantages such as the liquid phase nano particle stable in properties prepared.But laser liquid phase ablation is prepared noble metal nano structure and still be there is certain problem at present, the grain diameter as prepared is comparatively large and size is uneven first-class.
For above-mentioned technical problem, need badly and a kind of method can preparing stable, that size is controlled noble metal nano structure is provided.
Summary of the invention
For the deficiencies in the prior art, an object of the present invention is the preparation method providing a kind of noble metal nano structure, described method utilizes pulse laser ablation technology, using nano graphene oxide as seed promoters, prepares single dispersing noble metal nano structure in liquid phase.
The present invention utilizes the uniform noble metal nano structure of seed promoters mediated method controlled synthesis.The preparation method of nano material of seed promoters mediation refers to using certain material as seed nucleating point, induces material to be prepared to generate seed, then obtains the material of the nanostructured wanted.
The present invention is achieved through the following technical solutions:
The preparation method of noble metal nano structure is the solution be placed in by precious metal sheets containing nano graphene oxide, utilizes pulse laser to carry out ablation to precious metal sheets, obtains noble metal nano structure.
Noble metal of the present invention is selected from the combination of any a kind or at least 2 kinds in gold, silver, platinum; Preferred gold and/or platinum.
Preferably, purity >=90% of described precious metal sheets, such as 91%, 93%, 95%, 97% etc., preferably >=99.99%; .
Preferably, described precious metal sheets thickness is 0.5 ~ 5mm, such as 0.6mm, 0.7mm, 0.8mm etc., preferred 1mm.
Preferably, described precious metal sheets carries out machine glazed finish before use.
The concentration of nano graphene oxide solution of the present invention is 10 ~ 500 μ g/mL, such as 12 μ g/mL, 20 μ g/mL, 34 μ g/mL, 45 μ g/mL, 80 μ g/mL, 102 μ g/mL, 150 μ g/mL, 180 μ g/mL, 242 μ g/mL, 300 μ g/mL, 345 μ g/mL, 410 μ g/mL, 465 μ g/mL, 492 μ g/mL etc.
Preferably, the particle diameter of described nano graphene oxide is 1 ~ 20nm, such as 2nm, 5nm, 8nm, 12nm, 16nm, 19nm etc., preferably 1 ~ 2nm.
The wavelength of pulse laser of the present invention is 532nm or 1064nm, preferred 532nm.
Pulse laser generating means used in the present invention is typical but non-limiting is Nd:YAG pulse laser, and physical parameter is adjustable.
Preferably, the energy of described pulse laser is 30 ~ 400mJ, such as 35mJ, 42mJ, 95mJ, 135mJ, 250mJ, 350mJ etc., preferred 130mJ.The energy of described pulse laser can be adjusted by the voltage adjusting described pulse laser generating means.
Preferably, spot diameter≤2mm that described pulse laser focusing is formed in precious metal sheets surface, such as 0.5mm, 0.7mm, 1.2mm, 1.5mm, 1.8mm etc.
Preferably, the ablation time of described pulse laser is 5 ~ 60min, such as 7min, 30min, 47min, 55min, 59min etc., preferred 10min.
The preparation method of noble metal nano structure of the present invention comprises the steps:
(1) precious metal sheets is provided, and machine glazed finish is carried out to it, be placed in reaction vessel;
(2) nano graphene oxide solution is injected reaction vessel, and liquid level of solution do not have described precious metal sheets;
(3) pulse laser is through reaction vessel and nano graphene oxide solution, focuses on precious metal sheets surface, carries out ablation to precious metal sheets;
(4) solution in reaction vessel is separated by miillpore filter, afterwards through bag filter dialysis removing nano graphene oxide particle.
Reaction vessel material of the present invention is the combination of any a kind or at least 2 kinds in quartz, glass or plastics; Preferred quartz.
Preferably, described reaction vessel is preferably quartz ampoule.
Step of the present invention (3) described ablation is carried out in ultrasonic vibration.
The aperture of miillpore filter of the present invention is any a kind in 100nm, 220nm or 450nm, preferred 220nm;
Preferably, the molecular cut off of described bag filter is 3.5KD;
Preferably, described dialysis time is 1 ~ 24h, such as 3h, 13h, 17h, 23h etc.
Two of the object of the invention is to provide a kind of noble metal nano structure, and described noble metal nano structure is prepared by method as described in one of object.
The particle diameter of noble metal nano structure of the present invention is 2 ~ 5nm.
Three of the object of the invention is to provide a kind of purposes of noble metal nano structure as described in two of object, and described noble metal nano structure is applied to biomedical sector.
Compare the noble metal nano structure of chemical preparation, the product system of the noble metal nano structure that the liquid-phase pulse laser ablation that the present invention adopts prepares is pure, without other reagent that chemical reaction is brought into, and preparation technology is simple, reproducible, difference between batch is little, stable performance, colloidal state can be kept for a long time, and be beneficial to the modification of large biological molecule.
Compared with prior art, the present invention has following beneficial effect:
(1) the noble metal nano physical dimension prepared and pattern more homogeneous;
(2) size tunable of noble metal nano structure, along with the increase of nano graphene oxide seed promoters concentration, the size of gold nano structure is more and more less, and dispersiveness is also become better and better;
(3) the gold nano structural system prepared is pure, and without chemical residual, its good biocompatibility, for good basis is laid in the research afterwards at biomedical sector;
(4) preparation method is simple, and condition is easily controlled.
Accompanying drawing explanation
Fig. 1 is provided by the invention under the effect of nano graphene oxide seed promoters, adopts liquid-phase pulse laser ablation to obtain the schematic diagram of noble metal nano structure;
Fig. 2 is transmission electron microscope TEM image and the high-resolution-ration transmission electric-lens HRTEM image of gold nano structure prepared by embodiment 1; A is TEM image; B is HRTEM image;
Fig. 3 is the X-ray diffraction XRD token image of the gold nano structure prepared in 200mg/L nano graphene oxide seed promoters in embodiment 1;
Fig. 4 is the x-ray photoelectron spectroscopy XPS token image of the gold nano structure prepared in 200mg/L nano graphene oxide seed promoters in embodiment 1;
Fig. 5 is the TEM image of the gold nano structure of embodiment 1, embodiment 2 and embodiment 3 preparation; A is the TEM image of the gold nano structure of embodiment 1; B is the TEM image of the gold nano structure of embodiment 2; C is the TEM image of the gold nano structure of embodiment 3;
Fig. 6 is the TEM image of platinum nanostructured prepared by embodiment 4;
Fig. 7 is the Cytotoxic evaluation of gold nano structure prepared by embodiment 1;
Fig. 8 is the TEM image of the gold nano structure that comparative example 1 is prepared with embodiment 1; A is the TEM image of the gold nano structure of comparative example 1; B is the TEM image of the gold nano structure of embodiment 1.
Detailed description of the invention
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand, described embodiment is only help to understand the present invention, should not be considered as concrete restriction of the present invention.
The method preparing gold nano structure provided by the invention comprises the steps:
(1) precious metal sheets is provided, and machine glazed finish is carried out to it, be placed in reaction vessel;
(2) nano graphene oxide solution is injected reaction vessel, and liquid level of solution do not have described precious metal sheets;
(3) pulse laser is through reaction vessel and nano graphene oxide solution, focuses on precious metal sheets surface, carries out ablation to precious metal sheets;
(4) solution in reaction vessel is separated by miillpore filter, afterwards through bag filter dialysis removing nano graphene oxide particle.
Wherein, Fig. 1 is provided by the invention under the effect of nano graphene oxide seed promoters, adopts liquid-phase pulse laser ablation to obtain the schematic diagram of noble metal nano structure.
Embodiment 1
A preparation method for gold nano structure, comprises the steps:
(1) gold plaque is provided, and carries out machine glazed finish, be placed in reaction vessel; Described gold plaque purity is >=99.99wt%; Described gold plaque thickness is 1mm;
(2) be that the nano graphene oxide solution of 200mg/L injects reaction vessel by concentration, and liquid level did not have described gold plaque; Described nano graphene oxide is seed promoters; The particle diameter of nano graphene oxide is 1 ~ 2nm;
(3) provide a pulse laser generating means, the laser it produced guides in reaction vessel through optical path switching device, and focuses on gold plaque surface, carries out ablation to gold plaque;
Described pulse laser generating means is Nd:YAG pulse laser, and excitation wavelength is 532nm, pulse frequency 10Hz; Laser energy adjusts by adjusting the voltage of described pulse laser generating means, can weight range at 110 ~ 130mJ; Laser Focusing forms spot diameter≤2mm in gold plaque surface; The described ablation time is 10min;
(4) solution after pulse laser ablation is separated: the filtering with microporous membrane by the solution containing gold nano structure after step (3) pulse laser ablation through aperture being 220nm, be that the bag filter of 3.5KD is dialysed by filtrate molecular cut off, dialysis time is 12h, obtains product---gold nano structure.
The gold nano structure prepared embodiment 1 carries out transmission electron microscope TEM scanning and high-resolution-ration transmission electric-lens HRTEM scans, and scanning result is as Fig. 2 (Fig. 2 is transmission electron microscope TEM image and the high-resolution-ration transmission electric-lens HRTEM image of gold nano structure prepared by embodiment 1); The size of nanometer gold grain distribution prepared as can be seen from Figure 2 is between 1 ~ 5nm, and domain size distribution is more homogeneous, good dispersion; Find out that spacing of lattice 0.235nm is attributed to (111) crystal face of gold nano grain from high-resolution-ration transmission electric-lens HRTEM;
Carry out X-ray diffraction to the gold nano structure that embodiment 1 prepares, result is (Fig. 3 is the X-ray diffraction XRD token image of the gold nano structure of preparation in embodiment 1) as shown in Figure 3; As can be seen from Figure 3 gold nano grain (111) (200) (220) (311) characteristic of correspondence diffraction maximum;
Carry out x-ray photoelectron spectroscopy scanning to the gold nano structure that embodiment 1 prepares, result is (Fig. 4 is the x-ray photoelectron spectroscopy XPS token image of gold nano structure prepared by embodiment 1) as shown in Figure 4; The peak position at 4f7/2 and the 4f5/2 peak of x-ray photoelectron power spectrum display gold nano grain as can be seen from Figure 4.
Embodiment 2
A preparation method for gold nano structure, comprises the steps:
(1) gold plaque is provided, and carries out machine glazed finish, be placed in reaction vessel; Described gold plaque purity is >=99.99wt%; Described gold plaque thickness is 1mm;
(2) be that the nano graphene oxide solution of 40mg/L injects reaction vessel by concentration, and liquid level did not have described gold plaque; Described nano graphene oxide is seed promoters; The particle diameter of nano graphene oxide is 1 ~ 2nm;
(3) provide a pulse laser generating means, the laser it produced guides in reaction vessel through optical path switching device, and focuses on gold plaque surface, carries out ablation to gold plaque;
Described pulse laser generating means is Nd:YAG pulse laser, and excitation wavelength is 532nm, pulse frequency 10Hz; Laser energy adjusts by adjusting the voltage of described pulse laser generating means, can weight range at 110 ~ 130mJ; Laser Focusing forms spot diameter≤2mm in gold plaque surface; The described ablation time is 10min;
(4) solution after pulse laser ablation is separated: the filtering with microporous membrane by the solution containing gold nano structure after step (3) pulse laser ablation through aperture being 220nm, be that the bag filter of 3.5KD is dialysed by filtrate molecular cut off, dialysis time is 12h, obtain product---gold nano structure, its particle diameter is 3 ~ 9nm.
Embodiment 3
A preparation method for gold nano structure, comprises the steps:
(1) gold plaque is provided, and carries out machine glazed finish, be placed in reaction vessel; Described gold plaque purity is >=99.99wt%; Described gold plaque thickness is 1mm;
(2) be that the nano graphene oxide solution of 100mg/L injects reaction vessel by concentration, and liquid level did not have described gold plaque; Described nano graphene oxide is seed promoters; The particle diameter of nano graphene oxide is 1 ~ 2nm;
(3) provide a pulse laser generating means, the laser it produced guides in reaction vessel through optical path switching device, and focuses on gold plaque surface, carries out ablation to gold plaque;
Described pulse laser generating means is Nd:YAG pulse laser, and excitation wavelength is 532nm, pulse frequency 10Hz; Laser energy adjusts by adjusting the voltage of described pulse laser generating means, can weight range at 110 ~ 130mJ; It is≤2mm that Laser Focusing forms spot diameter in gold plaque surface; The described ablation time is 10min;
(4) solution after pulse laser ablation is separated: the filtering with microporous membrane by the solution containing gold nano structure after step (3) pulse laser ablation through aperture being 220nm, be that the bag filter of 3.5KD is dialysed by filtrate molecular cut off, dialysis time is 12h, obtain product---gold nano structure, its particle diameter is 3 ~ 6nm.
Carry out TEM scanning to the gold nano structure that embodiment 2 and embodiment 3 prepare, result is (Fig. 5 is the TEM image of the gold nano structure of embodiment 1, embodiment 2 and embodiment 3 preparation) as shown in Figure 5;
As can be seen from Figure 5, the concentration of nano graphene oxide particle is larger, and the size of nanometer gold grain prepared is less, and particle diameter is also more homogeneous.
Embodiment 4
A preparation method for platinum nanostructured, comprises the steps:
(1) platinized platinum is provided, and carries out machine glazed finish, be placed in reaction vessel; Described platinized platinum purity is >=99.99wt%; Described platinized platinum thickness is 1mm;
(2) be that the nano graphene oxide solution of 100mg/L injects reaction vessel by concentration, and liquid level did not have described platinized platinum; Described nano graphene oxide is seed promoters; The particle diameter of nano graphene oxide is 1 ~ 2nm;
(3) provide a pulse laser generating means, the laser it produced guides in reaction vessel through optical path switching device, and focuses on platinized platinum surface, carries out ablation to platinized platinum;
Described pulse laser generating means is Nd:YAG pulse laser, and excitation wavelength is 532nm, pulse frequency 10Hz; Laser energy adjusts by adjusting the voltage of described pulse laser generating means, can weight range at 110 ~ 130mJ; It is≤2mm that Laser Focusing forms spot diameter in gold plaque surface; The described ablation time is 10min;
(4) solution after pulse laser ablation is separated: the filtering with microporous membrane by the solution containing platinum nanostructured after step (3) pulse laser ablation through aperture being 220nm, be that the bag filter of 3.5KD is dialysed by filtrate molecular cut off, dialysis time is 12h, obtain product---platinum nanostructured, its particle diameter is 3 ~ 5nm.
Carry out TEM scanning to the platinum nanostructured that embodiment 4 prepares, result is (Fig. 6 is the TEM image of platinum nanostructured prepared by embodiment 4) as shown in Figure 6.
Embodiment 5
A preparation method for gold nano structure, is with the difference of embodiment 1, and the concentration of nano graphene oxide solution is 10 μ g/mL; The wavelength of pulse laser is 1064nm; The energy of described pulse laser is 300 ~ 400mJ; The ablation time of described pulse laser is 5min, and the gold nano structure particle diameter prepared is 5 ~ 10nm.
Embodiment 6
A preparation method for gold nano structure, is with the difference of embodiment 1, and the concentration of nano graphene oxide solution is 500 μ g/mL; The particle diameter of nano graphene oxide is 10 ~ 20nm; The energy of described pulse laser is 30 ~ 100mJ; The ablation time of described pulse laser is 60min, and the gold nano structure particle diameter prepared is 8 ~ 12nm.
Comparative example 1
A preparation method for gold nano structure, comprises the steps:
(1) gold plaque is provided, and carries out machine glazed finish, be placed in reaction vessel; Described gold plaque purity is >=99.99wt%; Described gold plaque thickness is 1mm;
(2) deionized water is injected reaction vessel, and liquid level do not have affiliated gold plaque;
(3) provide a pulse laser generating means, the laser it produced guides in reaction vessel through optical path switching device, and focuses on gold plaque surface, carries out ablation to gold plaque;
Described pulse laser generating means is Nd:YAG pulse laser, and excitation wavelength is 532nm, pulse frequency 10Hz; Laser energy adjusts by adjusting the voltage of described pulse laser generating means, can weight range at 110 ~ 130mJ; It is≤2mm that Laser Focusing forms spot diameter in gold plaque surface; The described ablation time is 10min;
Test case 1:
The gold nano structure that the gold nano structure provided with embodiment and comparative example 1 provide is object, tests to evaluate its cytotoxicity;
Method of testing:
(1) 100 μ L cell suspensions (every hole 1 × 10 in 96 orifice plates is prepared
4individual cell), and make it adherent;
(2) in 96 orifice plates, add the gold nano grain of variable concentrations respectively, make its final concentration gradient be 0.1 μ g/mL, 0.2 μ g/mL, 0.5 μ g/mL, 1 μ g/mL, 2 μ g/mL and 3 μ g/mL;
(3) 96 orifice plates are hatched 48 hours in incubator;
(4) add the CCK-8 solution that volume is 10 μ L in every hole, in incubator, hatch 2 hours;
(5) absorbance at 450nm place is measured with ELIASA;
(6) cell proliferation vigor is calculated.
Fig. 7 is the Cytotoxic evaluation of gold nano structure prepared by embodiment 1;
As can be seen from Figure 7, when gold nano grain is at 3mg/L, the survival rate of cell is still retained in about 80%; This shows, provided by the invention under the condition of graphene oxide solution as seed promoters, the biocompatibility of gold nano structure prepared by pulse laser ablation is relatively good, because gold grain surface is without any chemical modification, be convenient to the modification carrying out various large biological molecule as requested in the later stage uses, at biomedical sector, there is good potential application.
The gold nano grain that comparative example 1 and embodiment 1 obtain is carried out TEM scanning, and scanning result as shown in Figure 8; As can be seen from Figure 8, under nano graphene oxide does seed promoters mediated conditions, the size of gold nano structure is more homogeneous, and does not reunite, and dispersiveness is also better.
Applicant states, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, namely do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of auxiliary element, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (10)
1. a preparation method for noble metal nano structure, is characterized in that, described method is the solution be placed in by precious metal sheets containing nano graphene oxide, utilizes pulse laser to carry out ablation to precious metal sheets, obtains noble metal nano structure.
2. the method for claim 1, is characterized in that, described noble metal is selected from the combination of any a kind or at least 2 kinds in gold, silver, platinum; Preferred gold and/or platinum;
Preferably, purity >=90% of described precious metal sheets, preferably >=99.99%;
Preferably, described precious metal sheets thickness is 0.5 ~ 5mm, preferred 1mm;
Preferably, described precious metal sheets carries out machine glazed finish before use.
3. method as claimed in claim 1 or 2, it is characterized in that, the concentration of described nano graphene oxide solution is 10 ~ 500 μ g/mL;
Preferably, the particle diameter of described nano graphene oxide is 1 ~ 20nm, preferably 1 ~ 2nm.
4. the method as described in one of claims 1 to 3, is characterized in that, the wavelength of described pulse laser is 532nm or 1064nm, preferred 532nm;
Preferably, the energy of described pulse laser is 30 ~ 400mJ, preferred 130mJ;
Preferably, described pulse laser focusing is in the spot diameter≤2mm of precious metal sheets surface formation;
Preferably, the ablation time of described pulse laser is 5 ~ 60min, preferred 10min.
5. the method as described in one of Claims 1 to 4, is characterized in that, described method comprises the steps:
(1) precious metal sheets is provided, and machine glazed finish is carried out to it, be placed in reaction vessel;
(2) nano graphene oxide solution is injected reaction vessel, and liquid level of solution do not have described precious metal sheets;
(3) pulse laser is through reaction vessel and nano graphene oxide solution, focuses on precious metal sheets surface, carries out ablation to precious metal sheets;
(4) solution in reaction vessel is separated by miillpore filter, afterwards through bag filter dialysis removing nano graphene oxide particle.
6. method as claimed in claim 5, is characterized in that, described reaction vessel material is the combination of any a kind or at least 2 kinds in quartz, glass or plastics; Preferred quartz;
Preferably, described reaction vessel is preferably quartz ampoule.
7. the method as described in claim 5 or 6, is characterized in that, step (3) described ablation is carried out in ultrasonic vibration.
8. the method as described in one of claim 5 ~ 7, is characterized in that, the aperture of described miillpore filter is any a kind in 100nm, 220nm or 450nm, preferred 220nm;
Preferably, the molecular cut off of described bag filter is 3.5KD;
Preferably, described dialysis time is 1 ~ 24h.
9. a noble metal nano structure, is characterized in that, described noble metal nano structure is prepared by method as described in one of claim 1 ~ 8;
Preferably, the particle diameter of described noble metal nano structure is 2 ~ 5nm.
10. a purposes for noble metal nano structure as claimed in claim 9, it is characterized in that, described noble metal nano structure is applied to biomedical sector.
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