CN105921084A - Preparation method of core-shell structure cuprous oxide nano-composite - Google Patents
Preparation method of core-shell structure cuprous oxide nano-composite Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a preparation method of a core-shell structure cuprous oxide nano-composite. The preparation method includes the steps that seed nano-particle dispersion liquid is mixed with poly(diallyldimethylammonium chloride) with the molecular weight of 100000-200000, copper nitrate, sodium hydroxide and hydroxylamine hydrochloride, and thus a core@cuprous oxide nano-composite reaction precursor is obtained, wherein the seed nano-particle dispersion liquid is obtained by dispersing seed nano-particles serving as the core of a core-shell structure into a mixed solution of ethanediol and water; the core@cuprous oxide nano-composite reaction precursor reacts for 0.5-5 min at 0-100 DEG C, and thus the core@cuprous oxide nano-composite is obtained. The preparation method is simple in process, rapid, efficient and universally applicable to cores of different morphologies, compositions and structures; besides, the core-shell structure nano-composite with cuprous oxide serving as the coating shell can be prepared and is uniform in size, good in dispersity and excellent in optical absorption property.
Description
Technical field
The present invention relates to nuclear-shell structured nano-composite material field, particularly relate to a kind of nucleocapsid structure cuprous nano composite wood
The preparation method of material.
Background technology
Cuprous nano material is a kind of purposes Inorganic Chemicals widely, may be used for preparing coloring agent, catalysis
Agent, solder, preservative, marine antifouling coating, ballast, sensor, high-temperature superconductor etc., and cuprous nano
Material has superior photocatalysis performance and photoelectric transformation efficiency, and therefore it is led in area of solar cell and environmental pollution improvement
Territory is also with a wide range of applications.
In recent years, Composite, low-dimensional, intelligentized multifunctional nanocomposites are increasingly paid close attention to by people,
And the nano composite material of nucleocapsid structure is exactly the most representational one.Nucleocapsid structure is to be passed through by a kind of nano material
Another kind of nano material is coated with the ordered fabrication structure of the nanoscale formed that gets up by chemical bond or other active forces, generally adopts
Representing by the form of " a@b ", a therein is denoted as the nano material of nucleome, and b therein is denoted as being coated with shell
Nano material, such as: Ag@SiO2Represent with Ag nano-particle as nucleome, with SiO2For being coated with the nano material of shell.
In the prior art, have a lot with the preparation method that Red copper oxide is the nuclear-shell structured nano-composite material of cladding shell,
But these preparation methoies existing are difficult to prepare uniform particle diameter, the nuclear-shell structured nano-composite material of stable performance, and these are made
The most very complicated of Preparation Method, usual every kind of preparation method may be only available for a kind of nucleome, is not generally suitable for various nucleomes
Preparation method.
Summary of the invention
In order to solve above-mentioned technical problem of the prior art, the invention provides a kind of nucleocapsid structure cuprous nano and be combined
The preparation method of material, not only technique is simply, rapidly and efficiently, generally fit various different-shapes, composition, the nucleome of structure
With, and can prepare size uniformity, favorable dispersibility, absorbing properties excellent with Red copper oxide for cladding shell
Nuclear-shell structured nano-composite material.
It is an object of the invention to be achieved through the following technical solutions:
The preparation method of a kind of nucleocapsid structure cuprous nano composite, comprises the following steps:
Step A, by seed nanoparticulate dispersion and molecular weight be 100000～200000 polydiene base the third dimethylammonium chloride
Ammonium, copper nitrate, sodium hydroxide, oxammonium hydrochloride. mix, thus prepare core@cuprous nano composite precursors；
Wherein, described seed nanoparticulate dispersion is that the seed nano-particle as nucleocapsid structure nucleome is dispersed in ethylene glycol and water
In dispersion liquid in mixed solution, and the mixed solution of this ethylene glycol and water, the percent by volume of water is 20～80%；At core
In@cuprous nano composite precursors, the concentration of polydiene base the third alkyl dimethyl ammonium chloride is 0～0.2 mole/
Rise, the concentration of copper nitrate is 0.00005～0.01 mol/L, the concentration of sodium hydroxide is 0.0002～0.05 mol/L, salt
The concentration of acid azanol is 0.00005～0.02 mol/L.
Step B, described core@cuprous nano composite precursors is reacted 0.5～5 minute at 0～100 DEG C,
Thus prepare core@cuprous nano composite.
Preferably, in core@cuprous nano composite precursors, the concentration of seed nano-particle be 0.0001～
0.005 mol/L, the concentration of polydiene base the third alkyl dimethyl ammonium chloride are that 0.005～0.2 mol/L, the concentration of copper nitrate are
0.00005～0.01 mol/L, the concentration of sodium hydroxide are that 0.0002～0.05 mol/L, the concentration of oxammonium hydrochloride. are
0.00005～0.02 mol/L.
Preferably, in described step B, reaction temperature is 0～50 DEG C.
Preferably as nucleocapsid structure nucleome seed nano-particle first with the rotating speed of 3000～14500 revs/min carry out 5～
The centrifugal treating of 100 minutes, redispersion to ethylene glycol, with the mixed solution of water, forms seed nanoparticulate dispersion.
Preferably, the core@cuprous nano composite prepared step B with the rotating speed of 3000～14500 revs/min enters
Row 5～the centrifugal treating of 100 minutes, then use cleaning solvent to be carried out, thus prepare clean core@cuprous nano
Composite.
Preferably, described cleaning solvent uses one or more in deionized water, distilled water, dehydrated alcohol.
Preferably, by the concentration of copper nitrate in core@cuprous nano composite precursors is adjusted, from
And control the thickness of Red copper oxide shell in nucleocapsid structure.
As seen from the above technical solution provided by the invention, the nucleocapsid structure Red copper oxide that the embodiment of the present invention is provided is received
The preparation method of nano composite material uses seed mediated growth method oxammonium hydrochloride. reduction containing polydiene base the third alkyl dimethyl ammonium chloride nitre
Acid copper, seed nano-particle, ethylene glycol and the mixed solution of water of sodium hydroxide, be applicable to such that it is able to prepare with any shape
Looks, composition, structure nano-particle as the core@cuprous nano composite of nucleocapsid structure nucleome.By to core@
In cuprous nano composite precursors, the concentration of copper nitrate is adjusted, and can control the final core@oxygen prepared
Change the thickness of Red copper oxide shell in cuprous nano composite material.As can be seen here, the present invention not only technique simply, rapidly and efficiently,
Various different-shapes, composition, the nucleome of structure are generally suitable for, and can prepare size uniformity, favorable dispersibility,
The nuclear-shell structured nano-composite material being cladding shell with Red copper oxide that absorbing properties is excellent.
Accompanying drawing explanation
In order to be illustrated more clearly that the technical scheme of the embodiment of the present invention, in describing embodiment below, required use is attached
Figure is briefly described, it should be apparent that, the accompanying drawing in describing below is only some embodiments of the present invention, for ability
From the point of view of the those of ordinary skill in territory, on the premise of not paying creative work, it is also possible to obtain other according to these accompanying drawings attached
Figure.
Fig. 1 makes in the embodiment of the present invention 3 step a3 respectively for using NEC JEOL-1400 transmission electron microscope
The golden@cuprous nano composite wood prepared in the aubergine gold nano octahedron obtained and the embodiment of the present invention 3 step d3
The nano-particle of material is observed and is shot, thus the transmission electron microscope photo obtained (i.e. TEM figure).
Fig. 2 is for using Japan's Shimadzu UV-3101PC type ultraviolet-visible-near infrared spectrometer respectively to the present invention
The golden@prepared in the aubergine gold nano octahedron prepared in embodiment 1 step a1 and the embodiment of the present invention 1 step d1
The nano-particle of cuprous nano composite carries out quantitative test, thus the optical absorption map obtained.
Fig. 3 for use NEC JEOL-1400 transmission electron microscope respectively to the embodiment of the present invention 1, embodiment 2,
The golden@cuprous nano composite that embodiment 3 and embodiment 4 are finally prepared is observed and is shot, thus obtain
Transmission electron microscope photo (i.e. TEM figure).
Fig. 4 receives to gold nano bipyramid, gold@silver respectively for using NEC JEOL-1400 transmission electron microscope
Rice cubic block, gold@Silver nanorod, nano silver wire are as nucleome and according to the core@obtained by preparation method provided by the present invention
Cuprous nano composite is observed and is shot, thus the transmission electron microscope photo obtained (i.e. TEM figure).
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely retouched
State, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based on this
Bright embodiment, the every other enforcement that those of ordinary skill in the art are obtained under not paying creative work premise
Example, broadly falls into protection scope of the present invention.
Below the preparation method of nucleocapsid structure cuprous nano composite provided by the present invention is described in detail.
The preparation method of a kind of nucleocapsid structure cuprous nano composite, comprises the steps:
Step A, by seed nanoparticulate dispersion and molecular weight be 100000～200000 polydiene base the third dimethylammonium chloride
Ammonium, copper nitrate, sodium hydroxide, oxammonium hydrochloride. mix, thus prepare core@cuprous nano composite precursors.
Wherein, described seed nanoparticulate dispersion be the seed nano-particle as nucleocapsid structure nucleome be dispersed in ethylene glycol with
In dispersion liquid in the mixed solution of water, and the mixed solution of this ethylene glycol and water, the percent by volume of water is 20～80%.
Various patterns in prior art, various composition, various structure can be used as the seed nano-particle of nucleocapsid structure nucleome
Nano-particle, such as: various patterns, the gold nano grain of structure, various patterns, the silver nano-grain of structure, carbon ball is received
Rice grain, oxide nano particles etc..Seed nano-particle prepared by methods various in prior art can be present in respectively
Plant in different systems, therefore to avoid these systems that the present invention is produced impact, if seed nano-particle is not dispersion
In the ethylene glycol mixed solution with water (this ethylene glycol is 20～80% with the percent by volume of water in the mixed solution of water),
So seed nano-particle as nucleocapsid structure nucleome preferably first carries out 5～100 with the rotating speed of 3000～14500 revs/min
Minute centrifugal treating, redispersion to ethylene glycol, with the mixed solution of water, thus makes the seed nanometer meeting demand of the present invention
Particle dispersion.
Specifically, in core@cuprous nano composite precursors, polydiene base the third alkyl dimethyl ammonium chloride dense
Degree be 0～0.2 mol/L, the concentration of copper nitrate be 0.00005～0.01 mol/L, the concentration of sodium hydroxide be 0.0002～
0.05 mol/L, the concentration of oxammonium hydrochloride. are 0.00005～0.02 mol/L.In actual applications, described core@oxidation Asia
In copper nano composite material precursors, the concentration of seed nano-particle is preferably 0.0001～0.005 mol/L, polydiene
The concentration of base the third alkyl dimethyl ammonium chloride is preferably 0.005～0.2 mol/L, the concentration of copper nitrate is preferably 0.00005～0.01
Mol/L, the concentration of sodium hydroxide are preferably 0.0002～0.05 mol/L, the concentration of oxammonium hydrochloride. be preferably 0.00005～
0.02 mol/L.
Step B, by described core@cuprous nano composite precursors, at 0～100 DEG C, (reaction temperature is best
It is 0～50 DEG C) react 0.5～5 minute, thus prepare core@cuprous nano composite (i.e. Core@Cu2O nanometer
Composite).
Specifically, after step B completes, core@oxidation Asia step B prepared with the rotating speeds of 3000～14500 revs/min
Copper nano composite material carries out the centrifugal treating of 5～100 minutes, then use cleaning solvent (described cleaning solvent use go from
One or more in sub-water, distilled water, dehydrated alcohol) the green precipitate thing after centrifugal treating is carried out, thus can
To prepare clean core@cuprous nano composite.
Further, compared with the preparation method of nucleocapsid structure cuprous nano composite in prior art, the present invention is extremely
Have the advantage that less
(1) preparation method provided by the present invention is by the nitre in core@cuprous nano composite precursors
The concentration of acid copper is adjusted, and can control the thickness of Red copper oxide shell in nucleocapsid structure such that it is able to effectively control core@oxygen
Change the size of cuprous nano composite material.In actual applications, can be according to the seed nano-particle as nucleocapsid structure nucleome
Size, controls the thickness of Red copper oxide shell in nucleocapsid structure, such that it is able to it is multiple to control obtained core@cuprous nano flexibly
The size of condensation material.
(2) preparation method provided by the present invention is generally applicable to pattern any in prior art, composition, the receiving of structure
Rice grain is as nucleocapsid structure nucleome.By preparation method provided by the present invention prepare with Red copper oxide for cladding shell
Nuclear-shell structured nano-composite material (i.e. core@cuprous nano composite), its particle scale is highly uniform, has excellent
Different absorbing properties, and there is in the solution such as water or ethylene glycol extraordinary dispersibility.
(3) core@cuprous nano composite not only productivity height, work are prepared by preparation method provided by the present invention
Skill simply, easily operate, and abundant raw material, be not required to special equipment, with low cost, be suitable for large-scale production.
In order to more clearly from show technical scheme provided by the present invention and produced technique effect, below with concrete real
Execute example the preparation method of nucleocapsid structure cuprous nano composite provided by the present invention is described in detail.
Embodiment 1
A kind of 80 nanometer gold@cuprous nano composites, use following steps to be prepared from:
Step a1, first by diallyl dimethyl ammoniumchloride (this diallyl dimethyl that Solute mass fraction is 20%
The molecular weight of ammonium chloride is 100000～200000) aqueous solution joins mix homogeneously in ethylene glycol, adds gold chloride water
Solution, making the concentration of diallyl dimethyl ammoniumchloride in this mixed solution is that 0.025 mol/L, the concentration of gold chloride are
0.0005 mol/L, then reacts 30 minutes at 220 DEG C, thus prepares the aubergine gold nano octahedral that yardstick is 60 nanometers
Body colloid solution.
Step b1, by step a1 prepare described gold nano octahedron colloid solution naturally cool to room temperature, then stir at magnetic force
In gold nano octahedron colloid solution, 18 megaohms of deionized waters, copper nitrate, sodium hydroxide and hydrochloric acid it is sequentially added under the conditions of mixing
Aqueous hydroxylamine solution, thus prepare core@cuprous nano composite precursors；Wherein, described core@Red copper oxide
In nano composite material precursors, the percent by volume of water is 50%, the concentration of copper nitrate is 0.00025 mol/L,
The concentration of sodium hydroxide be 0.02 mol/L, the concentration of oxammonium hydrochloride. be 0.01 mol/L.
Step c1, core@cuprous nano composite precursors step b1 prepared are under protective atmosphere and room temperature
React 0.5 minute, thus prepare gold@cuprous nano composite.
Step d1, by step c1 prepare golden@cuprous nano composite be placed in a centrifuge, with 10000 revs/min
Rotating speed carry out the centrifugal treating of 20 minutes, then use deionized water that the green precipitate thing after centrifugal treating is carried out 3～5 times
Ultrasonic cleaning, thus prepare clean green gold@cuprous nano composite.Through observation: the embodiment of the present invention 1
In the nano-particle of prepared golden@cuprous nano composite, the thickness of Red copper oxide shell is 10 nanometers, namely
Saying, the particle size of this gold@cuprous nano composite is 60+10+10=80 nanometer.
Embodiment 2
A kind of 100 nanometer gold@cuprous nano composites, use following steps to be prepared from:
Step a2, first by diallyl dimethyl ammoniumchloride (this diallyl dimethyl that Solute mass fraction is 20%
The molecular weight of ammonium chloride is 100000～200000) aqueous solution joins mix homogeneously in ethylene glycol, adds gold chloride water
Solution, making the concentration of diallyl dimethyl ammoniumchloride in this mixed solution is that 0.025 mol/L, the concentration of gold chloride are
0.0005 mol/L, then reacts 30 minutes at 220 DEG C, thus prepares the aubergine gold nano octahedral that yardstick is 60 nanometers
Body colloid solution.
Step b2, by step a2 prepare described gold nano octahedron colloid solution naturally cool to room temperature, then stir at magnetic force
In gold nano octahedron colloid solution, 18 megaohms of deionized waters, copper nitrate, sodium hydroxide and hydrochloric acid it is sequentially added under the conditions of mixing
Aqueous hydroxylamine solution, thus prepare core@cuprous nano composite precursors；Wherein, described core@Red copper oxide
In nano composite material precursors, the percent by volume of water is 50%, the concentration of copper nitrate is 0.0005 mol/L, hydrogen
The concentration of sodium oxide be 0.02 mol/L, the concentration of oxammonium hydrochloride. be 0.01 mol/L.
Step c2, core@cuprous nano composite precursors step b2 prepared are under protective atmosphere and room temperature
React 0.5 minute, thus prepare gold@cuprous nano composite.
Step d2, by step c2 prepare golden@cuprous nano composite be placed in a centrifuge, with 10000 revs/min
Rotating speed carry out the centrifugal treating of 20 minutes, then use deionized water that the green precipitate thing after centrifugal treating is carried out 3～5 times
Ultrasonic cleaning, thus prepare clean green gold@cuprous nano composite.Through observation: the embodiment of the present invention 2
In the nano-particle of prepared golden@cuprous nano composite, the thickness of Red copper oxide shell is 20 nanometers, namely
Saying, the particle size of this gold@cuprous nano composite is 60+20+20=100 nanometer.
Embodiment 3
A kind of 160 nanometer gold@cuprous nano composites, use following steps to be prepared from:
Step a3, first by diallyl dimethyl ammoniumchloride (this diallyl dimethyl that Solute mass fraction is 20%
The molecular weight of ammonium chloride is 100000～200000) aqueous solution joins mix homogeneously in ethylene glycol, adds gold chloride water
Solution, making the concentration of diallyl dimethyl ammoniumchloride in this mixed solution is that 0.025 mol/L, the concentration of gold chloride are
0.0005 mol/L, then reacts 30 minutes at 220 DEG C, thus prepares the aubergine gold nano octahedral that yardstick is 60 nanometers
Body colloid solution.
Step b3, by step a3 prepare described gold nano octahedron colloid solution naturally cool to room temperature, then stir at magnetic force
In gold nano octahedron colloid solution, 18 megaohms of deionized waters, copper nitrate, sodium hydroxide and hydrochloric acid it is sequentially added under the conditions of mixing
Aqueous hydroxylamine solution, thus prepare core@cuprous nano composite precursors；Wherein, described core@Red copper oxide
In nano composite material precursors, the percent by volume of water is 50%, the concentration of copper nitrate is 0.001 mol/L, hydrogen
The concentration of sodium oxide be 0.02 mol/L, the concentration of oxammonium hydrochloride. be 0.01 mol/L.
Step c3, core@cuprous nano composite precursors step b3 prepared are under protective atmosphere and room temperature
React 0.5 minute, thus prepare gold@cuprous nano composite.
Step d3, by step c3 prepare golden@cuprous nano composite be placed in a centrifuge, with 10000 revs/min
Rotating speed carry out the centrifugal treating of 20 minutes, then use deionized water that the green precipitate thing after centrifugal treating is carried out 3～5 times
Ultrasonic cleaning, thus prepare clean green gold@cuprous nano composite.Through observation: the embodiment of the present invention 3
In the nano-particle of prepared golden@cuprous nano composite, the thickness of Red copper oxide shell is 50 nanometers, namely
Saying, the particle size of this gold@cuprous nano composite is 60+50+50=160 nanometer.
Embodiment 4
A kind of 180 nanometer gold@cuprous nano composites, use following steps to be prepared from:
Step a4, first by diallyl dimethyl ammoniumchloride (this diallyl dimethyl that Solute mass fraction is 20%
The molecular weight of ammonium chloride is 100000～200000) aqueous solution joins mix homogeneously in ethylene glycol, adds gold chloride water
Solution, making the concentration of diallyl dimethyl ammoniumchloride in this mixed solution is that 0.025 mol/L, the concentration of gold chloride are
0.0005 mol/L, then reacts 30 minutes at 220 DEG C, thus prepares the aubergine gold nano octahedral that yardstick is 60 nanometers
Body colloid solution.
Step b4, by step a4 prepare described gold nano octahedron colloid solution naturally cool to room temperature, then stir at magnetic force
In gold nano octahedron colloid solution, 18 megaohms of deionized waters, copper nitrate, sodium hydroxide and hydrochloric acid it is sequentially added under the conditions of mixing
Aqueous hydroxylamine solution, thus prepare core@cuprous nano composite precursors；Wherein, described core@Red copper oxide
In nano composite material precursors, the percent by volume of water is 50%, the concentration of copper nitrate is 0.002 mol/L, hydrogen
The concentration of sodium oxide be 0.02 mol/L, the concentration of oxammonium hydrochloride. be 0.01 mol/L.
Step c4, core@cuprous nano composite precursors step b4 prepared are under protective atmosphere and room temperature
React 0.5 minute, thus prepare gold@cuprous nano composite.
Step d4, by step c4 prepare golden@cuprous nano composite be placed in a centrifuge, with 10000 revs/min
Rotating speed carry out the centrifugal treating of 20 minutes, then use deionized water that the green precipitate thing after centrifugal treating is carried out 3～5 times
Ultrasonic cleaning, thus prepare clean green gold@cuprous nano composite.Through observation: the embodiment of the present invention 4
In the nano-particle of prepared golden@cuprous nano composite, the thickness of Red copper oxide shell is 60 nanometers, namely
Saying, the particle size of this gold@cuprous nano composite is 60+60+60=180 nanometer.
The pattern of embodiment 1～4 and performance detection
Respectively the embodiment of the present invention 1, embodiment 2, embodiment 3 and the golden@cuprous nano prepared by embodiment 4 are combined
Material detects, thus obtains following result:
(1) use NEC JEOL-1400 transmission electron microscope respectively in the embodiment of the present invention 3 step a3 prepare
Receiving of the golden@cuprous nano composite prepared in aubergine gold nano octahedron and the embodiment of the present invention 3 step d3
Rice grain is observed and is shot, thus obtains transmission electron microscope photo (i.e. TEM figure) as shown in Figure 1；Wherein, Fig. 1 a
For the aubergine gold nano octahedral low power TEM figure prepared in the embodiment of the present invention 3 step a3；Fig. 1 b is that the present invention implements
The aubergine gold nano octahedral high power TEM figure prepared in example 3 step a3；Fig. 1 c is in the embodiment of the present invention 3 step d3
The low power TEM figure of the nano-particle of the golden@cuprous nano composite prepared；Fig. 1 d is the embodiment of the present invention 3 step
The high power TEM figure of the nano-particle of the golden@cuprous nano composite prepared in d3.By Fig. 1 a, Fig. 1 b, Fig. 1 c
With Fig. 1 d it can be seen that the nanometer of golden@cuprous nano composite that finally prepares of the embodiment of the present invention 3 step d3
Grain be yardstick uniform nucleocapsid structure Heterogeneous Composite nanoparticle, granular size be 160 nanometers, and productivity is the highest, as core
The gold nano of body octahedra complete oxidized cuprous shell parcel, the octahedral length of side of gold nano is 60 nanometers, and Red copper oxide shell
Thickness is 50 nanometers.
(2) use Japan's Shimadzu UV-3101PC type ultraviolet-visible-near infrared spectrometer real to the present invention respectively
Execute the golden@oxidation prepared in the aubergine gold nano octahedron and the embodiment of the present invention 1 step d1 prepared in example 1 step a1
The nano-particle of cuprous nano composite material carries out quantitative test, thus obtains optical absorption map as shown in Figure 2；Wherein,
The vertical coordinate of Fig. 2 is absorption intensity, and the abscissa of Fig. 2 is optical wavelength.As can be seen from Figure 2: described gold nano is octahedra
Absworption peak in 560 nanometers；The nano-particle of described gold@cuprous nano composite has the strongest in 635 nanometers
Optical absorption characteristics；Compared with described gold nano octahedron, the absworption peak red shift of described gold@cuprous nano composite
75 nanometers, absorption intensity is octahedral 1.8 times of described gold nano, therefore has the present invention of above-mentioned excellent optical absorption characteristics
The golden@cuprous nano composite that embodiment 1 finally prepares is at aspects such as surface-enhanced Raman, biochemistry sensings all
It is with a wide range of applications.
(3) use NEC JEOL-1400 transmission electron microscope respectively to the embodiment of the present invention 1, embodiment 2, reality
Execute example 3 and golden@cuprous nano composite that embodiment 4 is finally prepared is observed and shot, thus obtain such as Fig. 3
Shown transmission electron microscope photo (i.e. TEM figure)；Wherein, Fig. 3 a is the golden@oxidation Asia that the embodiment of the present invention 1 is finally prepared
The TEM figure of the nano-particle of copper nano composite material；Fig. 3 b is that the golden@Red copper oxide that the embodiment of the present invention 2 is finally prepared is received
The TEM figure of the nano-particle of nano composite material；Fig. 3 c is that the golden@cuprous nano that the embodiment of the present invention 3 is finally prepared is multiple
The TEM figure of the nano-particle of condensation material；Fig. 3 d is the golden@cuprous nano composite wood that the embodiment of the present invention 4 is finally prepared
The TEM figure of the nano-particle of material.By Fig. 3 a, Fig. 3 b, Fig. 3 c and Fig. 3 d it can be seen that preparation side provided by the present invention
Method, can be on a large scale by being adjusted the copper nitrate concentration in core@cuprous nano composite precursors
The thickness of Red copper oxide shell in the nucleocapsid structure of interior Effective Regulation end product.
Embodiment 5
Respectively using gold nano bipyramid in prior art, gold@silver nanoparticle cubic block, gold@Silver nanorod, nano silver wire as
Nucleocapsid structure nucleome, and use preparation method provided by the present invention preparation to receive with Red copper oxide for the nucleocapsid structure of cladding shell
Nano composite material.NEC JEOL-1400 transmission electron microscope is used to receive to gold nano bipyramid, gold@silver respectively
Rice cubic block, gold@Silver nanorod, nano silver wire are seen as the core@cuprous nano composite prepared by nucleome
Examine and shoot, thus obtain transmission electron microscope photo as shown in Figure 4；Wherein, Fig. 4 a is with gold nano bipyramid as nuclear regime
The TEM figure of the golden@cuprous nano composite obtained；Fig. 4 b is the golden@obtained for nuclear regime with gold@silver nanoparticle cubic block
The TEM figure of silver@cuprous nano composite；Fig. 4 c is the golden@silver@oxidation obtained for nuclear regime with gold@Silver nanorod
The TEM figure of cuprous nano composite material；Fig. 4 d is the silver-colored@cuprous nano composite obtained for nuclear regime with nano silver wire
TEM figure.By Fig. 4 a, Fig. 4 b, Fig. 4 c and Fig. 4 d it can be seen that preparation method provided by the present invention can be with difference
Pattern, composition, the nano-particle of structure prepare different composition, pattern, the core Red copper oxide nucleocapsid of structure as nucleome
Heterogeneous Composite nanoparticle.
As fully visible, the embodiment of the present invention not only technique simply, rapidly and efficiently, to various different-shapes, composition, structure
Nucleome is generally suitable for, and can prepare size uniformity, favorable dispersibility, absorbing properties excellent with Red copper oxide be
The nuclear-shell structured nano-composite material of cladding shell.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto, and appoints
How those familiar with the art is in the technical scope that the invention discloses, the change that can readily occur in or replacement, all
Should contain within protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection domain of claims
It is as the criterion.
Claims (7)
1. the preparation method of a nucleocapsid structure cuprous nano composite, it is characterised in that comprise the following steps:
Step A, by seed nanoparticulate dispersion and molecular weight be 100000～200000 polydiene base the third dimethylammonium chloride
Ammonium, copper nitrate, sodium hydroxide, oxammonium hydrochloride. mix, thus prepare core@cuprous nano composite precursors；
Wherein, described seed nanoparticulate dispersion be the seed nano-particle as nucleocapsid structure nucleome be dispersed in ethylene glycol with
In dispersion liquid in the mixed solution of water, and the mixed solution of this ethylene glycol and water, the percent by volume of water is 20～80%；
In core@cuprous nano composite precursors, the concentration of polydiene base the third alkyl dimethyl ammonium chloride is 0～0.2 to rub
You/liter, the concentration of copper nitrate be 0.00005～0.01 mol/L, the concentration of sodium hydroxide be 0.0002～0.05 mol/L,
The concentration of oxammonium hydrochloride. is 0.00005～0.02 mol/L；
Step B, described core@cuprous nano composite precursors is reacted 0.5～5 minute at 0～100 DEG C,
Thus prepare core@cuprous nano composite.
Preparation method the most according to claim 1, it is characterised in that react at core@cuprous nano composite
In presoma, the concentration of seed nano-particle is 0.0001～0.005 mol/L, the concentration of polydiene base the third alkyl dimethyl ammonium chloride
Be 0.005～0.2 mol/L, the concentration of copper nitrate be 0.00005～0.01 mol/L, the concentration of sodium hydroxide be 0.0002～
0.05 mol/L, the concentration of oxammonium hydrochloride. are 0.00005～0.02 mol/L.
Preparation method the most according to claim 1 and 2, it is characterised in that in described step B, reaction temperature be 0～
50℃。
Preparation method the most according to claim 1 and 2, it is characterised in that as the seed nanometer of nucleocapsid structure nucleome
Granule first carries out the centrifugal treating of 5～100 minutes, redispersion to ethylene glycol and water with the rotating speed of 3000～14500 revs/min
Mixed solution in, form described seed nanoparticulate dispersion.
Preparation method the most according to claim 1 and 2, it is characterised in that with the rotating speed of 3000～14500 revs/min
The core@cuprous nano composite preparing step B carries out the centrifugal treating of 5～100 minutes, then uses cleaning solvent
It is carried out, thus prepares clean core@cuprous nano composite.
Preparation method the most according to claim 5, it is characterised in that described cleaning solvent uses deionized water, steaming
One or more in distilled water, dehydrated alcohol.
Preparation method the most according to claim 1 and 2, it is characterised in that by core@cuprous nano is combined
In material precursors, the concentration of copper nitrate is adjusted, thus controls the thickness of Red copper oxide shell in nucleocapsid structure.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107584135A (en) * | 2017-08-31 | 2018-01-16 | 中国科学院合肥物质科学研究院 | A kind of method for quickly preparing three-dimensional porous electrum nano material |
| CN115055678A (en) * | 2022-05-25 | 2022-09-16 | 北京信息科技大学 | Preparation method of gold particle-cuprous oxide nanometer cup |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102350499A (en) * | 2011-09-28 | 2012-02-15 | 河北工业大学 | Cu/Cu2O core-shell composite microsphere and preparation method thereof |
| US20150291778A1 (en) * | 2014-04-09 | 2015-10-15 | The Shepherd Color Company | Core-shell composite inorganic metal oxides and method of preparing for prevention of thermal oxidative degradation in polymer and resin compositions |
-
2016
- 2016-04-29 CN CN201610291220.3A patent/CN105921084A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102350499A (en) * | 2011-09-28 | 2012-02-15 | 河北工业大学 | Cu/Cu2O core-shell composite microsphere and preparation method thereof |
| US20150291778A1 (en) * | 2014-04-09 | 2015-10-15 | The Shepherd Color Company | Core-shell composite inorganic metal oxides and method of preparing for prevention of thermal oxidative degradation in polymer and resin compositions |
Non-Patent Citations (5)
| Title |
|---|
| HAO JING ET AL.: "Epitaxial Growth of Cu2O on Ag Allows for Fine Control Over Particle Geometries and Optical Properties of Ag-Cu2O Core-Shell Nanoparticles", 《THE JOURNAL OF PHYSICAL CHEMISTRY C》 * |
| NOGA MEIR ET AL.: "Studying the chemical, optical and catalytic properties of noble metal (Pt, Pd, Ag, Au)–Cu2O core–shell nanostructures grown via a general approach", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
| SHIH-CHEN HSU ET AL.: "Facet-Dependent Surface Plasmon Resonance Properties of Au–Cu2O Core–Shell Nanocubes, Octahedra, and Rhombic Dodecahedra", 《MATERIALS VIEWS》 * |
| YIQIANG SUN ET AL.: "Complete Au@ZnO core–shell nanoparticles with enhanced plasmonic absorption enabling significantly improved photocatalysis", 《NANOSCALE》 * |
| YU-CHEN YANG ET AL.: "Facet-dependent optical properties of polyhedral Au–Cu2O core–shell nanocrystals", 《NANOSCALE》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107584135A (en) * | 2017-08-31 | 2018-01-16 | 中国科学院合肥物质科学研究院 | A kind of method for quickly preparing three-dimensional porous electrum nano material |
| CN107584135B (en) * | 2017-08-31 | 2019-04-09 | 中国科学院合肥物质科学研究院 | A method of quickly preparing three-dimensional porous gold-silver alloy nano material |
| CN115055678A (en) * | 2022-05-25 | 2022-09-16 | 北京信息科技大学 | Preparation method of gold particle-cuprous oxide nanometer cup |
| CN115055678B (en) * | 2022-05-25 | 2023-06-27 | 北京信息科技大学 | Preparation method of gold particle-cuprous oxide nano cup |
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