CN106807940A - Collaurum/di-iron trioxide core-shell type nano structural composites and preparation method thereof - Google Patents
Collaurum/di-iron trioxide core-shell type nano structural composites and preparation method thereof Download PDFInfo
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- CN106807940A CN106807940A CN201510845952.8A CN201510845952A CN106807940A CN 106807940 A CN106807940 A CN 106807940A CN 201510845952 A CN201510845952 A CN 201510845952A CN 106807940 A CN106807940 A CN 106807940A
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- collaurum
- core
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- iron
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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 kind of collaurum/di-iron trioxide core-shell type nano structural composites and preparation method thereof.The preparation method includes：Collaurum containing quaternary cationic surfactant is provided, and add alkaline matter make the collaurum in alkalescence, source of iron is added afterwards, it is reacted that the collaurum/di-iron trioxide core-shell type nano structural composites are obtained, the shell of the compound has even mesoporous structure, and the source of iron includes the molysite containing organic matter part.The compound includes collaurum core and coats the di-iron trioxide shell of the collaurum core, and the shell has even mesoporous structure.Preparation method of the invention a step can be completed at normal temperatures, and simple to operate, repetitive rate is high, and product yield is high, and morphology controllable, energy consumption is low, and the nontoxic solvent used in building-up process does harm to, safety and environmental protection, it is adaptable to mass produce.
Description
Technical field
The present invention relates to a kind of hud typed composite nano materials, more particularly to a kind of collaurum/di-iron trioxide core-shell type nano knot
Structure compound and preparation method thereof.
Background technology
Nano composite material is made up of two or more nano materials, is subject to extensive due to its unique property and technique application
Concern.Collaurum and ferric oxide nano composite are a focuses of current research, and gold-iron oxide composite nanostructure has
Unique optics and magnetic performance, has good application prospect on biomedical sector and catalytic field.Nano composite structure
Middle core shell structure and dumbbell shape structure are the most famous, its relative to the material of wherein single component have more preferable optics, magnetics and
Catalytic performance.
The research of current coreshell type structure focuses mostly in collaurum/di-iron trioxide shell structure, and its technology of preparing is always a tool
Challenging research work.So far, the synthetic technology of collaurum core/di-iron trioxide shell composite nanostructure is mainly
Self-assembly method and coprecipitation in situ.Wherein self-assembling method is divided into three steps, including：The first step, be respectively synthesized gold nanorods and
Di-iron trioxide nano particle；Second step, in the appropriate organic ligand of gold nanorods surface modification；3rd step, after modification
Gold nanorods and ferric oxide particle are mixed, ferric oxide particles be adsorbed onto gold nanorods surface formed gold nanorods core/
Di-iron trioxide shell core-shell type nano structure.Coprecipitation method in situ is divided into two steps, including：The first step, synthesizes gold nano star
And in its surface modification polyvinylpyrrolidone；Second step, original position co-precipitation ferrous iron and ferric iron source synthesize nano combined knot
Structure.Self-assembly method building-up process mainly has three aspects in the presence of inevitable shortcoming：First, the oxidation two of pyrolyzing synthesis nanometer three
The temperature of iron particle is up to 260 DEG C, and energy consumption is very big, and the time is long；Second, by repeatedly in the modification to gold nanorods
Centrifuge washing material loss it is big, easily reunite；3rd, the nanostructured that synthetic product is inlayed for ferric oxide particle, rather than
Complete nucleocapsid structure.Coprecipitation in situ except excessive material loss can be produced in modification, outside the defect such as easily reunite,
It is major disadvantage is also that be difficult to form porous crust.
The content of the invention
In view of the shortcomings of the prior art, it is a primary object of the present invention to provide a kind of collaurum/di-iron trioxide core-shell type nano
Structural composites and preparation method thereof.
To realize aforementioned invention purpose, the technical solution adopted by the present invention includes：
An embodiment provides a kind of preparation side of collaurum/di-iron trioxide core-shell type nano structural composites
Method, it includes：Collaurum containing quaternary cationic surfactant is provided, and adds the alkaline matter to make the collaurum be in
Alkalescence, adds source of iron afterwards, and the reacted prepared collaurum/di-iron trioxide core-shell type nano structural composites are described multiple
The shell of compound has even mesoporous structure, and the source of iron includes the molysite containing organic matter part.
An embodiment provides a kind of collaurum/di-iron trioxide core-shell type nano structural composites, it includes glue
The di-iron trioxide shell of body gold core and the cladding collaurum core, the shell has even mesoporous structure.
Compared with prior art, advantages of the present invention includes：
(1) the synthesis work of collaurum/di-iron trioxide core-shell type nano structural composites is prepared there is provided a kind of simple one-step method
Skill, its is simple to operate, and repetitive rate is high, and a step can complete at normal temperatures, in greatly reducing energy loss, and building-up process
The solvent for using is water and a small amount of methyl alcohol or ethanol, and safety non-toxic evil is suitable for large-scale production；
(2) in the collaurum for being obtained/di-iron trioxide core-shell type nano structural composites, collaurum core is coated on di-iron trioxide
In shell structurre, and shell is non-particulate for uniform meso-hole structure, while the yield of the compound is high, pattern and shell are thick
Degree is easily controlled.
Brief description of the drawings
Fig. 1 is a kind of synthesis of collaurum/di-iron trioxide core-shell type nano structural composites in a typical embodiments of the invention
Process chart；
Fig. 2 is the transmission electron microscope picture of the AuNR (gold nanorods) using seed law growth in the embodiment of the present invention 1；
Fig. 3 is AuNR@Fe in the embodiment of the present invention 12O3(gold nanorods/di-iron trioxide core-shell type nano structure composite
Thing) transmission electron microscope picture；
Fig. 4 is AuNR and AuNR@Fe in the embodiment of the present invention 12O3Ultraviolet-visible absorption spectroscopy figure；
Fig. 5 is AuNP@Fe in the embodiment of the present invention 22O3(gold nano grain/di-iron trioxide core-shell type nano structure composite
Thing) transmission electron microscope picture；
Fig. 6 is AuNS@Fe in the embodiment of the present invention 32O3(gold nano star/di-iron trioxide core-shell type nano structure composite
Thing) transmission electron microscope picture；
Fig. 7 is AuNP (gold nano grain), AuNP@Fe in embodiment of the present invention 2- embodiments 32O3, AuNS (Jenners
Rice star particle) and AuNS@Fe2O3Ultraviolet-visible absorption spectroscopy figure.
Specific embodiment
In view of deficiency of the prior art, inventor is able to propose technical side of the invention through studying for a long period of time and largely putting into practice
Case.The technical scheme, its implementation process and principle etc. will be further explained as follows.
One aspect of the present invention provides a kind of preparation method of collaurum/di-iron trioxide core-shell type nano structural composites,
It includes：Collaurum containing quaternary ammonium salt cationic surfactant (such as cetyl trimethylammonium bromide) is provided, and adds basic species
Matter makes the collaurum in alkalescence, and source of iron is added afterwards, reacted that the collaurum/di-iron trioxide core-shell type nano knot is obtained
Structure compound, the shell of the compound has even mesoporous structure, and the source of iron includes the molysite containing organic matter part.
More preferred, golden nanometer particle and the mol ratio of cetyl trimethylammonium bromide are 1 in the collaurum：
1.8×10-6~9 × 10-6。
More preferred, the concentration of golden nanometer particle is 0.7~0.9nM in the collaurum.Wherein " nM " is also denoted as
“nmol/L”。
More preferred, described preparation method includes：The pH value of the collaurum is adjusted to using alkaline matter
9.5~11.5.
More preferred, the alkaline matter includes the combination of any one or more in NaOH, ammoniacal liquor, but is not limited to
This.
More preferred, the source of iron is 1 × 10 with the molar ratio range of golden nanometer particle in the collaurum5~5.6 × 105：
1。
More preferred, the source of iron is the organic solution of the molysite containing organic matter part, organic molten in the organic solution
Agent includes any one in methyl alcohol, ethanol, isopropanol, acetone or two or more combinations, but not limited to this.
More preferred, the source of iron includes the combination of any one or more in ferric acetyl acetonade, ferric acetate, but is not limited to
This.
One aspect of the present invention provides a kind of collaurum/di-iron trioxide core-shell type nano structural composites, and it includes colloid
The di-iron trioxide shell of golden core and the cladding collaurum core, the shell has even mesoporous structure.
Further, the particle diameter of the collaurum core is 15~300nm.
Further, the di-iron trioxide shell thickness is 5~30nm.
Further, the aperture of contained hole is 2~10nm in the even mesoporous structure of the shell.
Further, the collaurum core includes gold nano grain (AuNP), gold nanorods (AuNR), gold nano star
(AuNS) any one and in nanometer Golden Triangle or two or more combinations, but not limited to this.
Fig. 1 is refer to, in one more specific embodiment, a kind of collaurum/di-iron trioxide core-shell type nano structure composite
The preparation method of thing includes：
(1) after taking collaurum high speed centrifugation, the washing of a certain amount of cetyl trimethylammonium bromide stabilization, with deionization moisture
Dissipate, the collaurum after being concentrated；
(2) take the collaurum after concentration to be dissipated with moisture, be subsequently adding cetyl trimethylammonium bromide, wherein by control ten
The amount of six alkyl trimethyl ammonium bromides can control the pattern of di-iron trioxide shell；
(3) pH value for adding the regulation solution such as sodium hydrate aqueous solution is alkalescence, such as pH value=10；
(4) methanol solution of appropriate ferric acetyl acetonade is dividedly in some parts, for example, every 10-50 microlitres of addition in 1 hour, plus
Reaction system keeps concussion or magnetic agitation state during entering；
(5) fully reaction, obtains collaurum/di-iron trioxide core-shell type nano structure after acetylacetone,2,4-pentanedione ferrous solution is added and terminated,
Wherein the thickness of di-iron trioxide shell can be controlled by controlling the amount of addition acetylacetone,2,4-pentanedione ferrous solution.
Make detailed explanation to technical scheme below in conjunction with drawings and Examples.
1 gold nanorods of embodiment/di-iron trioxide core-shell type nano structural composites (AuNR@Fe2O3Material) preparation
(1) (pattern refers to figure to take 10 milliliters of gold nanorods (concentration about 0.9nM) of cetyl trimethylammonium bromide stabilization
2), 7000 revs/min, it is centrifuged 30 minutes, centrifugation twice, is subsequently adding the dispersion of 1 ml deionized water.
(2) collaurum after 500 microlitres of concentrations is taken, plus 3.235 milliliters of moisture dissipate, and are subsequently adding the 16 of about 0.1 mol/L
0~19 microlitre of the alkyl trimethyl ammonium bromide aqueous solution.
(3) pH value for adding sodium hydrate aqueous solution regulation solution is 10.
(4) 40~200 microlitres of the methanol solution of the ferric acetyl acetonade of concentration about 0.02M is added, 10-50 was added every 1 hour
Microlitre, reaction system keeps concussion or magnetic agitation state in adition process.
(5) acetylacetone,2,4-pentanedione ferrous solution reacts 2 hours or so after adding and terminating, and obtains AuNR Fe2O3Material, its pattern can
Refering to Fig. 3, the aperture averaging of its contained hole is about 3.2nm, and shell average thickness is about 13.91nm, and its UV, visible light
Absorption spectrum is as shown in Figure 4.
2 gold nano grains of embodiment/di-iron trioxide core-shell type nano structural composites (AuNP@Fe2O3Material) preparation
(1) the gold nano grain average grain diameter for taking 10 milliliters of cetyl trimethylammonium bromide stabilizations is 31nm, 7000 revs/min
Clock, is centrifuged 30 minutes, and centrifugation twice, is subsequently adding the dispersion of 1 ml deionized water.
(2) collaurum after 500 microlitres of concentrations is taken, plus 3.235 milliliters of moisture dissipate, and are subsequently adding the hexadecane of 0.1 mol/L
0~19 microlitre of the base trimethylammonium bromide aqueous solution.
(3) pH value for adding sodium hydrate aqueous solution regulation solution is 10.
(4) 40~200 microlitres of the methanol solution of the ferric acetyl acetonade of concentration about 0.02M is added, 10-50 was added every 1 hour
Microlitre, reaction system keeps concussion or magnetic agitation state in adition process.
(5) acetylacetone,2,4-pentanedione ferrous solution reacts 2 hours or so after adding and terminating, and obtains AuNP Fe2O3Material, its pattern can
Refering to Fig. 5, and its ultraviolet-visible absorption spectroscopy is as shown in Figure 7.
The gold nano star of embodiment 3/di-iron trioxide core-shell type nano structural composites (AuNS@Fe2O3Material) preparation
(1) the gold nano star average grain diameter for taking 10 milliliters of cetyl trimethylammonium bromide stabilizations is 68.4nm, 7000 revs/min
Clock, is centrifuged 30 minutes, and centrifugation twice, is subsequently adding the dispersion of 1 ml deionized water.
(2) collaurum after 500 microlitres of concentrations is taken, plus 3.235 milliliters of moisture dissipate, and are subsequently adding the hexadecane of 0.1 mol/L
0~19 microlitre of the base trimethylammonium bromide aqueous solution.
(3) pH value for adding sodium hydrate aqueous solution regulation solution is 10.
(4) 40~200 microlitres of the methanol solution of the ferric acetyl acetonade of concentration about 0.02M is added, 10-50 was added every 1 hour
Microlitre, reaction system keeps concussion or magnetic agitation state in adition process.
(5) acetylacetone,2,4-pentanedione ferrous solution reacts 2 hours or so after adding and terminating, and obtains AuNS Fe2O3Material, its pattern can
Refering to Fig. 6, and its ultraviolet-visible absorption spectroscopy is as shown in Figure 7.
It is with the shell structurre of the source of iron synthesis containing organic matter part in collaurum core of the invention/di-iron trioxide shell nanostructured
Uniform meso-hole structure, synthetic method repetitive rate is high, simple easily operated, synthesizes under normal temperature, and solvent is water, methyl alcohol or ethanol
Deng, safety non-toxic, the sample yield of synthesis is high, and the pattern and shell thickness of product are easily controlled, relative to prior art synthesize
Cost is relatively low, is more suitable for industrialization production.
It should be appreciated that above-described embodiment is only explanation technology design of the invention and feature, technique is familiar with its object is to allow
Personage will appreciate that present disclosure and implement according to this that it is not intended to limit the scope of the present invention.It is all according to this hair
The equivalent change or modification that bright Spirit Essence is made, should all be included within the scope of the present invention.
Claims (10)
1. the preparation method of a kind of collaurum/di-iron trioxide core-shell type nano structural composites, it is characterised in that including：There is provided
Collaurum containing quaternary cationic surfactant, and add alkaline matter make the collaurum in alkalescence, iron is added afterwards
Source, reacted that the collaurum/di-iron trioxide core-shell type nano structural composites are obtained, the shell of the compound has
Even meso-hole structure, the source of iron includes the molysite containing organic matter part.
2. preparation method according to claim 1, it is characterised in that：
Golden nanometer particle and the mol ratio of quaternary cationic surfactant are 1 in the collaurum：1.8×10-6~9 × 10- 6；
And/or, the concentration range of golden nanometer particle is 0.7~0.9nmol/L in the collaurum；
And/or, the quaternary cationic surfactant includes cetyl trimethylammonium bromide.
3. preparation method according to claim 1, it is characterised in that including：Using alkaline matter by the collaurum
PH value is adjusted to 9.5~11.5.
4. according to the preparation method of claim 1 or 3, it is characterised in that：The alkaline matter is included in NaOH and ammoniacal liquor
The combination of any one or two kinds.
5. preparation method according to claim 1, it is characterised in that：The source of iron and golden nanometer particle in the collaurum
Mol ratio be 1 × 105~5.6 × 105：1.
6. preparation method according to claim 1, it is characterised in that：The source of iron is the molysite containing organic matter part
Organic solution, organic solvent in the organic solution includes any one or two in methyl alcohol, ethanol, isopropanol, acetone
Plant combination of the above.
7. the preparation method according to claim 1,5 or 6, it is characterised in that：The source of iron include ferric acetyl acetonade and
The combination of any one or two kinds in ferric acetate.
8. a kind of collaurum/di-iron trioxide core-shell type nano structural composites, it is characterised in that including collaurum core and cladding
The di-iron trioxide shell of the collaurum core, the shell has even mesoporous structure.
9. collaurum according to claim 8/di-iron trioxide core-shell type nano structural composites, it is characterised in that：
The particle diameter of the collaurum core is 10~300nm；
And/or, the di-iron trioxide shell thickness is 5~30nm；
And/or, the aperture of contained hole is 2~10nm in the even mesoporous structure of the shell.
10. collaurum according to claim 8/di-iron trioxide core-shell type nano structural composites, it is characterised in that described
Collaurum core includes gold nano grain, gold nanorods, any one in gold nano star and nanometer Golden Triangle or two or more groups
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| US20110250122A1 (en) * | 2008-11-07 | 2011-10-13 | The Regents Of The University Of California | Core-Shell Nanocatalyst For High Temperature Reactions |
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| CN103528996A (en) * | 2013-10-11 | 2014-01-22 | 南京邮电大学 | Preparation method of gold nanorod SPR probe and method for detecting drug loading release kinetic process of the probe |
| CN104128199A (en) * | 2014-07-08 | 2014-11-05 | 东南大学 | Nano-gold catalyst and preparation method thereof |
| CN104707998A (en) * | 2015-03-13 | 2015-06-17 | 盐城工学院 | Nanometer golden rod used for detecting bovine serum albumin and preparation method and application thereof |
| CN105036070A (en) * | 2015-06-30 | 2015-11-11 | 国家纳米科学中心 | Gold nanorod-silicon dioxide core-shell structure nanometer material, preparation method and application |
-
2015
- 2015-11-27 CN CN201510845952.8A patent/CN106807940B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110250122A1 (en) * | 2008-11-07 | 2011-10-13 | The Regents Of The University Of California | Core-Shell Nanocatalyst For High Temperature Reactions |
| CN102672169A (en) * | 2012-06-07 | 2012-09-19 | 北京科技大学 | Method for preparing gold/titanium dioxide core-shell nanoparticle |
| CN102896312A (en) * | 2012-11-02 | 2013-01-30 | 厦门大学 | Metal/iron oxide nano material with core-shell structure and preparation method thereof |
| CN103528996A (en) * | 2013-10-11 | 2014-01-22 | 南京邮电大学 | Preparation method of gold nanorod SPR probe and method for detecting drug loading release kinetic process of the probe |
| CN104128199A (en) * | 2014-07-08 | 2014-11-05 | 东南大学 | Nano-gold catalyst and preparation method thereof |
| CN104707998A (en) * | 2015-03-13 | 2015-06-17 | 盐城工学院 | Nanometer golden rod used for detecting bovine serum albumin and preparation method and application thereof |
| CN105036070A (en) * | 2015-06-30 | 2015-11-11 | 国家纳米科学中心 | Gold nanorod-silicon dioxide core-shell structure nanometer material, preparation method and application |
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