CN106141171A - Hud typed superstructure nano material, its preparation method and application - Google Patents
Hud typed superstructure nano material, its preparation method and application Download PDFInfo
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- CN106141171A CN106141171A CN201510202658.5A CN201510202658A CN106141171A CN 106141171 A CN106141171 A CN 106141171A CN 201510202658 A CN201510202658 A CN 201510202658A CN 106141171 A CN106141171 A CN 106141171A
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Abstract
The invention discloses a kind of hud typed superstructure nano material, its preparation method and application.This hud typed superstructure nano material is to be formed, comprising: provide the nano metal material as nucleus, and at described nano metal material surface modified high molecular by a kind of novel noncontinuity regrowth pattern preparation；Surface is modified with high molecular described nano metal material and inserts in selective solvent, make polymer segment collapse or stretch, thus form discrete, to be available for the second metal accumulation nano-area at nucleating surface；And make bimetallic atom pile up formation superstructure in the nano-area noncontinuity of described nucleating surface.The preparation method of the present invention is simple to operation, and controllability is good, and is obtained hud typed superstructure nano material and have excellent properties, and obtained multistage Au/Pd superstructure nano material has very high surface electro-chemical activity, can be used for highly sensitive detection H2O2Deng material.
Description
Technical field
The present invention relates to the preparation method of a kind of core-shell structured nanomaterials, utilize noncontinuity regrowth pattern particularly to one
Prepare method of hud typed superstructure nano material (the superstructure bimetal nano material such as such as Au/Pd) and application thereof, such as
Application in sensing detection field.
Background technology
The physics of nano material, particularly metal nanoparticle, chemical property are by its size, composition, crystallinity, shape and knot
The impact of structure is the biggest.Wherein, the synthesis that shape controls has become an importance in metal nanoparticle research.The most often
A kind of method seen is the growing method of seed modulation.Such as, in an exemplary embodiments, the method is: first water-soluble
Liquid obtains the spherical gold grain of a few nanosized, referred to as crystal seed by strong reductant reduction gold salt；Afterwards gold salt, structure are led
Mix with certain proportion to the aqueous solution of agent (such as cetyl trimethylammonium bromide) and weak reductant (such as ascorbic acid), be referred to as to make a living
Long solution；Finally, in growth solution, the least gold nano grain is added as nuclearing centre, variously-shaped gold nano knot
Structure will be formed.
Tradition core-shell structured nanomaterials research in, surfactant in noble metal nano particles building-up process, all right and wrong
Covalent bond absorption is at nucleating surface, and when the metallic atom being reduced piles up nucleating surface, the surfactant of physical absorption is competing
Striving replacement, then adsorb in outermost nanoparticle surface, this continuous growth pattern typically prepares continuous print shell structurre, and
More difficult acquisition morphology controllable, discrete shell structurre.Such as, refer to be i.e. to use nanometer gold bar as crystalline substance shown in Fig. 1 a
Core, and utilize tradition seriality nucleus regrowth pattern to prepare the schematic diagram of hud typed Au/Pd nano material.
Summary of the invention
A kind of hud typed superstructure nano material of offer and noncontinuity regrowth pattern preparation side thereof are provided
Method, thus overcome deficiency of the prior art.
Another object of the present invention is to provide the purposes of described hud typed superstructure nano material.
For realizing aforementioned invention purpose, the technical solution used in the present invention includes:
A kind of hud typed superstructure nano material, comprising:
As the nano metal material being made up of the first metal nucleus, main,
And, as the superstructure formed in the discontinuous growth of described nucleating surface by the second metal shell, main.
Further, described first metal the most certainly but is not limited to Au.
Further, described second metal the most certainly but is not limited to Pt, Pd, Ag.
Further, described nucleus the most certainly but is not limited to the nano-particle that particle diameter is 3nm～100nm.
Further, the shape of described nano-particle is at least selected from bar-shaped, spherical, cubic.
Further, described superstructure includes that Discrete Distribution is in plural nano-particle (the particularly mean diameter of described nucleating surface
Extra small nano-particle at below 5nm), described nano-particle is mainly made up of the second metal.
Wherein, if described superstructure is spherical, then its size can regulate and control between 50-150nm；And for cuboid
Superstructure, its length can regulate and control between 50-250nm, and diameter is about between 20-100nm.
Further, the particle diameter of described hud typed superstructure nano material is preferably 20nm～200nm.
Among an embodiment, described hud typed superstructure nano material is bimetallic multilevel superstructure nano material, Qi Zhongjing
Core and shell are made up of the first metal, the second metal respectively.
A kind of method preparing described hud typed superstructure nano material, comprising:
Nano metal material as nucleus is provided, and modifies selected macromolecule on described nano metal material surface,
Surface is modified with selected high molecular described nano metal material and inserts in selective solvent, make selected polymer segment collapse
Contracting or stretching, extension, thus form discrete, to be available for the second metal accumulation nano-area at nucleating surface,
And, make bimetallic atom pile up formation superstructure in the nano-area noncontinuity of described nucleating surface.
Among one more preferred embodiment, described preparation method may include that and makes selected high score by chemical bonding mode
Son is modified described nano metal material surface.
Wherein, described selected macromolecule can be hydrophobic polymer, such as, can be polymethyl methacrylate or polystyrene,
But it is not limited to this, and corresponding selective solvent is water, polar organic solvent etc..
Contrary, if described selected macromolecule is hydrophilic macromolecule, such as polyvinyl alcohol, polyacrylic acid, Polyethylene Glycol etc.,
Then corresponding selective solvent is non-polar solven or weak polar solvent.
Among one more preferred embodiment, described preparation method may include that by by bimetallic ion reduction shape
Become atom and be deposited in described nucleating surface and form superstructure.
Any one the hud typed superstructure nano material aforementioned application in preparation detection kit or sensor.
Such as, providing a kind of sensing element among an application scheme, it comprises described hud typed superstructure nano material.
Such as, among an application scheme, a kind of H is provided2O2Detection probe, it comprises superstructure Au/Pd nano material, institute
State multilevel superstructure Au/Pd nano material include Au nano-particle and main by Discrete Distribution at Au nano grain surface
The superstructure of Pd nano-particle composition.
This H2O2Detection probe is for H2O2Detection limit can as little as 1 μM.
Further, wherein Pd granule system is the Pd nanometer rods of super-small, and it is ordered in gold nanorods surface as shell.
The present invention is tied to nucleating surface by chemical bond (such as S-Au, gold-sulfide linkage) macromolecule, stops by newly-generated metal
Atom competition is replaced, thus forms a kind of noncontinuity nucleating surface growth being different from conventional precious metal particle growth mode
Pattern, the most exposed nucleating surface is available for being realized continued growth by atom packing space.According to this novel growth pattern,
The metal nanoparticle (such as gold nano grain) of different-shape is selected as nucleus, and chemical bond is passed through by macromolecule in its surface
Binding, in selective solvent, the macromolecular chain of outer layer is collapsed to nucleating surface, forms a noncontinuity growing surface (example
Such as noncontinuity reduction growing surface) so that it is its metal or non-metallic atom can grow at these discrete nucleating surfaces, enter
And hud typed superstructure nano material can be formed, the particularly super nano structural material of bimetallic nucleocapsid.
Compared with prior art, beneficial effect of the present invention at least that:
(1) the noncontinuity growth pattern that polymer chemistry provided by the present invention modification nucleus causes is a kind of novel synthetic kernel
The method of many metal hybrids nano material of shell mould superstructure nano material, particularly new multistage structure, it is simple to operation,
And in operation, can very easily regulate and control the component of nano material, pattern (only needing to adjust the pattern of nucleus) etc.；
(2) the hud typed superstructure nano material that the present invention is obtained has many premium properties, and superstructure is due to the chi of nanoparticle
Very little effect and the coupling effect of multicomponent nanocomposite metal, can produce special optics, electricity and catalytic performance.The most therein
Multilevel superstructure Au/Pd nano material has very high surface electro-chemical activity, is applicable as highly sensitive detection sensing nano material, and
And have bright prospects in fields such as preparing efficient food sensor.
Accompanying drawing explanation
Fig. 1 a-Fig. 1 b is in the regrowth schematic diagram of conventional ion SURFACTANT ADSORPTION gold core and the present invention one case study on implementation respectively
The noncontinuity growth pattern schematic diagram formed by the nucleus of chemical bond binding modified ligand；
Fig. 2 is the noncontinuity growth pattern system that in one embodiment of the invention, the nanometer gold bar nucleus of polymer chemistry key binding is formed
The transmission electron microscope photo of standby golden palladium (Au/Pd) superstructure nano material；
Fig. 3 is the golden palladium superstructure nanometer material formed using ball-type nanometer gold as the discontinuous growth of nucleus in another embodiment of the present invention
The transmission electron microscope picture of material；
Fig. 4 is the golden palladium superstructure nanometer formed using Cubic nanometer gold as the discontinuous growth of nucleus in further embodiment of this invention
The transmission electron microscope picture of material；
Fig. 5 a-Fig. 5 b is the high-resolution elementary analysis TEM picture of gold palladium superstructure nano material shown in Fig. 4；
Fig. 6 is with the cyclic voltammetry curve figure of the detection hydrogen peroxide of gold palladium superstructure nano material shown in Fig. 4.
Detailed description of the invention
The present invention is substantially for the deficiencies in the prior art, it is provided that the noncontinuity regrowth mould of a kind of novel nano material
Formula, utilizes this pattern can obtain novel hud typed superstructure nano material.
In some case study on implementation of the present invention, gold nano grain, such as nanometer gold bar, gold goal or Gionee cube all can be chosen
As nucleus, by binding modified ligand macromolecule in its surface chemistry, and selective solvent is utilized to make the macromolecular chain of its outer layer
It is collapsed to gold rod surface, forms other metallic atom that a noncontinuity is available for being reduced, the nanometer table of such as palladium atom packing
Face, and then make palladium atom noncontinuity be stacked into gold nano grain surface, form gold palladium (Au/Pd) superstructure nano material etc..
In more specifically among embodiment of the present invention, primary gold nano can be formed by electronation gold chloride in the solution
Particle, as nucleus, prepares the gold nano grain of the different-shapes such as ball-type, rod type, cubic type by controlling reaction condition, it
After, refer to Fig. 1 b, can add in Pd ion growth-promoting media after gold nano grain surface chemistry binding macromolecule, preparation gold palladium
Superstructure nano material.
Further, this embodiment may include steps of:
(1) preparation of the gold nano grain of different-shape
The gold nano grain of different-shape, as ball-type, rod, Cubic can serve as modifying nucleus.Ball with 18nm particle diameter
As a example by type nanometer gold nucleus, by 100mL, 2.5 × 10-4The chlorauric acid solution of M is heated to 120 DEG C, adds the lemon of 10mL 1wt%
Lemon acid sodium solution, after heated and stirred 20min, solution colour becomes claret, prepares the gold nano grain of about 18nm.Take 10
ML gold nano grain solution, centrifugal 10min (8000pm), and again it is dispersed in the cetyl trimethyl of 10mL, 80mM
In the aqueous solution of ammonium bromide (CTAB) standby.
(2) gold nano grain surface chemical modification hydrophobic polymer
Hydrophobic polymer containing sulfydryl is used for the surface of chemical modification gold nano grain, such as polymethyl methacrylate, polyphenyl
Ethylene etc..Here, as a example by 6-sulfydryl hex-1-alcohol (MCH), again divide after centrifugal for 20mL gold nano grain seed solution
It is dispersed in 20mL dimethylformamide (DMF), 100mg MCH is dissolved in 2mL DMF, join 20mL gold nano
In the DMF solution of particle, 24h is stirred at room temperature, after centrifugal purification, the Au@MCH of acquisition is dispersed in DMF standby again.
(3) gold nano grain surface in situ reduction growth Pd nano particle
1mL Au@MCH solution is joined 5-20mL 0.001M H2PdCl4Aqueous solution in, ultrasonic 1min uniformly divides
Dissipate, be then quickly added in the ascorbic acid solution of 1-5mL, 0.01M, be stirred vigorously 10s ambient temperatare and put more than 6h, thus
Prepare gold palladium superstructure nano material.
Make to illustrate in more detail to technical scheme below in conjunction with some embodiments and accompanying drawing.
Embodiment 1: the preparation of bar-shaped gold palladium superstructure nano material, comprises the steps:
(1) bar-shaped gold nano seed is prepared
The preparation of nanometer gold seed: by the 5 × 10 of 10mL-4The HAuCl of M4Solution joins the 0.2M CTAB of 10mL
In (cetyl trimethylammonium bromide) solution, then by the ice-cold NaBH of 1.2mL4Solution (0.01M) rapidly joins
In above-mentioned mixed solution, it is stirred vigorously 2min.After left at room temperature at least 10min standby.The preparation of gold ion growth-promoting media: by 4
The HAuCl of mL4(0.01M) with 0.8mL AgNO3Solution (0.01M) joins in the CTAB solution (0.1M) of 80mL
It is sufficiently mixed, and the ascorbic acid solution (0.1M) of 0.64mL is added in growth-promoting media, be uniformly mixed, add 1.6mL
The pH value of 1.0M dilute hydrochloric acid solution growth regulation liquid.Then the nanometer gold seed solution of 0.02mL is rapidly joined growth-promoting media
In, stirring 10s, ambient temperatare prepares gold nanorods after putting 6h.Centrifugal 10min under 8000rpm, by the gold nanorods weight of precipitation
New dispersion is the most standby.
(2) gold nanorods surface chemistry binding macromolecule
Hydrophobic polymer MCH containing sulfydryl is used for the surface of the gold nanorods of chemical modification, by the gold nanorods kind of 20mL
Again it is dispersed in after sub-solution centrifugal in 20mL solvent dimethylformamide (DMF), 100mg MCH is dissolved in 2mL DMF
In, join in the DMF solution of 20mL gold nanorods, 24h is stirred at room temperature, after centrifugal purification by obtained Au@MCH again
It is dispersed in DMF standby.
(3) bar-shaped gold palladium superstructure nano material is prepared
1mL Au@MCH solution is joined 5mL 0.001M H2PdCl4Aqueous solution in, ultrasonic 1min is dispersed, so
After rapidly join in the ascorbic acid solution of 1mL, 0.01M, be stirred vigorously 10s ambient temperatare and put more than 6h.Thus prepare gold palladium
Superstructure nano material, its pattern refers to Fig. 2.
Embodiment 2: the preparation of ball-type Au/Pd superstructure nano material, comprises the steps:
(1) spherical gold nano seed is prepared
By 100mL, 2.5 × 10-4The chlorauric acid solution of M is heated to 120 DEG C, adds 10mL, the sodium citrate solution of 1%, adds
After thermal agitation 20min, solution colour becomes claret, prepares the gold nanosphere of about 18nm.Take 10mL gold nanosphere solution,
It is centrifuged in 10min (8000pm), and the aqueous solution of the cetyl ammonium bromide being again dispersed in 10mL, 80mM standby.
(2) gold nanosphere surface chemistry binding macromolecule
Hydrophobic polymer MCH containing sulfydryl is used for the surface of chemical modification gold nanosphere, by molten for 20mL gold nanosphere seed
Again it is dispersed in 20mL solvent dimethylformamide (DMF) after liquid is centrifugal, 100mg MCH is dissolved in 2mL DMF,
Join in the DMF solution of 20mL gold nanosphere, 24h is stirred at room temperature, after centrifugal purification, obtained Au@MCH is dispersed in again
In DMF standby.
(3) spherical gold palladium superstructure nano material is prepared
1mL Au@MCH solution is joined 5mL 0.001M H2PdCl4Aqueous solution in, ultrasonic 1min is dispersed, so
After rapidly join in the ascorbic acid solution of 1mL, 0.01M, be stirred vigorously 10s ambient temperatare and put more than 6h.Thus prepare gold palladium
Superstructure nano material, its pattern refers to Fig. 3.
Embodiment 3: the preparation of bar-shaped Au/Pd superstructure nano material, comprises the steps:
(1) Cubic gold nano seed is prepared
The HAuCl4 solution of the 0.01M of 0.25mL is joined in the 0.1M CTAB solution of 7.5mL, then by 0.6mL
Ice-cold NaBH4 solution (0.01M) rapidly joins in above-mentioned mixed solution, is stirred vigorously 2min.Left at room temperature at least 1h
The most standby.The preparation of gold ion growth-promoting media: by the CTAB solution (0.1M) of the HAuCl4 (0.01M) and 6.4mL of 0.8mL
Join in 32mL deionized water and be sufficiently mixed, and the ascorbic acid solution (0.1M) of 3.8mL is added in growth-promoting media, stir
Mix mix homogeneously.Then rapidly joining in growth-promoting media by the nanometer gold seed solution of 0.02mL, stir 10s, ambient temperatare puts 6h
Rear prepared Cubic gold nano grain (also known as gold nano cube).Centrifugal 10min under 8000rpm, by the gold nano of precipitation
Grain disperses the most standby again.
(2) gold nano cube face chemistry binding macromolecule
Hydrophobic polymer MCH containing sulfydryl is used for the surface of chemical modification gold nano grain, by 20mL gold nano grain kind
Again it is dispersed in after sub-solution centrifugal in 20mL solvent dimethylformamide (DMF), 100mg MCH is dissolved in 2mL DMF
In, join in the DMF solution of 20mL golden nanometer particle, 24h is stirred at room temperature, after centrifugal purification by obtained Au@MCH again
It is dispersed in DMF standby.
(3) cubic gold palladium superstructure nano material is prepared
1mL Au@MCH solution is joined 5mL 0.001M H2PdCl4Aqueous solution in, ultrasonic 1min is dispersed, so
After rapidly join in the ascorbic acid solution of 1mL, 0.01M, be stirred vigorously 10s ambient temperatare and put more than 6h.Thus prepare gold palladium
Superstructure nano material, its pattern refers to Fig. 4, and high-resolution TEM of its elementary analysis refer to Fig. 5 a-Fig. 5 b.
The super nanostructured of this gold palladium (Au/Pd) nucleocapsid can be applicable to highly sensitive detection hydrogen peroxide (H2O2), it detects performance
Refer to Fig. 6 (detection limit can as little as 1 μM).
Should be appreciated that above is only to have much representational several embodiment, to the present invention in the numerous concrete exemplary applications of the present invention
Protection domain do not constitute any limitation.The technical scheme that all employing equivalents or equivalence are replaced and formed, all falls within this
Within the scope of bright rights protection.
Claims (10)
1. a hud typed superstructure nano material, it is characterised in that including:
As the nano metal material being made up of the first metal nucleus, main,
And, as the superstructure formed in the discontinuous growth of described nucleating surface by the second metal shell, main.
Hud typed superstructure nano material the most according to claim 1, it is characterised in that described first metal includes Au,
Described second metal includes Pt, Pd or Ag.
Hud typed superstructure nano material the most according to claim 1 and 2, it is characterised in that described nucleus selected from particle diameter is
The nano-particle of 3nm～100nm, the shape of described nano-particle is at least selected from bar-shaped, spherical, cubic.
Hud typed superstructure nano material the most according to claim 1 and 2, it is characterised in that described superstructure includes discrete
Being distributed in the nano-particle of described nucleating surface, described nano-particle is mainly made up of the second metal.
Hud typed superstructure nano material the most according to claim 1, it is characterised in that described hud typed superstructure nanometer material
The particle diameter of material is 20nm～200nm.
6. the preparation method of hud typed superstructure nano material as according to any one of claim 1-5, it is characterised in that including:
Nano metal material as nucleus is provided, and modifies selected macromolecule on described nano metal material surface,
Surface is modified with selected high molecular described nano metal material and inserts in selective solvent, make selected polymer segment collapse
Contracting or stretching, extension, thus form discrete, to be available for the second metal accumulation nano-area at nucleating surface；
And, make bimetallic atom pile up formation superstructure in the nano-area noncontinuity of described nucleating surface.
The preparation method of hud typed superstructure nano material the most according to claim 6, it is characterised in that including: by changing
Learning bonding pattern makes selected macromolecule be modified described nano metal material surface.
The preparation method of hud typed superstructure nano material the most according to claim 6, it is characterised in that including: by inciting somebody to action
Bimetallic ion reduction forms atom and is deposited in described nucleating surface and forms superstructure.
9. the hud typed superstructure nano material according to any one of claim 1-5 is in preparation detection kit or sensor
Application.
10. a H2O2Detection probe, it is characterised in that comprising superstructure Au/Pd nano material, described superstructure Au/Pd is received
Rice material includes Au nano-particle and the superjunction being mainly made up of at the Pd nano-particle of Au nano grain surface Discrete Distribution
Structure.
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| CN110038562A (en) * | 2019-04-25 | 2019-07-23 | 中国科学技术大学 | A kind of catalyst and its preparation method and application |
| CN110183742A (en) * | 2019-05-17 | 2019-08-30 | 浙江大学 | A kind of laminated film and preparation method and application of the multicolour variation of stress response |
| CN110202163A (en) * | 2019-05-21 | 2019-09-06 | 山东理工大学 | A kind of preparation method of Ag@Au@Pd nano cubic hollow shell structure |
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| CN108031840A (en) * | 2018-01-15 | 2018-05-15 | 国家纳米科学中心 | A kind of heterogeneous nano-superstructure of self-supporting metal and its preparation method and application |
| CN110038562A (en) * | 2019-04-25 | 2019-07-23 | 中国科学技术大学 | A kind of catalyst and its preparation method and application |
| CN110038562B (en) * | 2019-04-25 | 2020-06-26 | 中国科学技术大学 | Catalyst and preparation method and application thereof |
| CN110183742A (en) * | 2019-05-17 | 2019-08-30 | 浙江大学 | A kind of laminated film and preparation method and application of the multicolour variation of stress response |
| CN110183742B (en) * | 2019-05-17 | 2020-07-07 | 浙江大学 | Stress-responsive multicolor composite film and preparation method and application thereof |
| CN110202163A (en) * | 2019-05-21 | 2019-09-06 | 山东理工大学 | A kind of preparation method of Ag@Au@Pd nano cubic hollow shell structure |
| CN110202163B (en) * | 2019-05-21 | 2023-03-21 | 山东理工大学 | Preparation method of Ag @ Au @ Pd nano cubic hollow shell structure |
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