CN108237223A - Hud typed gold-ruthenium-oxide nanocomposite and preparation method thereof - Google Patents
Hud typed gold-ruthenium-oxide nanocomposite and preparation method thereof Download PDFInfo
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- CN108237223A CN108237223A CN201810025853.9A CN201810025853A CN108237223A CN 108237223 A CN108237223 A CN 108237223A CN 201810025853 A CN201810025853 A CN 201810025853A CN 108237223 A CN108237223 A CN 108237223A
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- 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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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
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Abstract
The present invention relates to a kind of hud typed golden ruthenium-oxide nanocomposite, gold nanoparticle including kernel and its external ruthenium-oxide is coated on, the molar ratio of gold nanoparticle and ruthenium-oxide is 1:0.2‑0.8.The present invention also provides the preparation methods of above-mentioned hud typed golden ruthenium-oxide nanocomposite, include the following steps：The pH value of gold-containing solution is adjusted to 8 12, add mixing after the organic solution of acetylacetone,2,4-pentanedione ruthenium, wherein described gold-containing solution includes gold nanoparticle, cationic surfactant and water, a concentration of the 0.05 × 10 of cationic surfactant in the gold-containing solution‑3‑1.5×10‑3mol/L；Mixed solution at 100 120 DEG C is subjected to hydro-thermal reaction, obtains hud typed golden ruthenium-oxide nanocomposite.Hud typed golden ruthenium-oxide nanocomposite is synthesized under the conditions of high temperature hydrothermal synthesis using simple one-step method, easy to operate, repetitive rate is high, and the product yield of synthesis is high, and pattern and shell thickness are easily controllable.
Description
Technical field
The present invention relates to technical field of nanometer material preparation more particularly to a kind of hud typed nano combined materials of gold-ruthenium-oxide
Material and preparation method thereof.
Background technology
Due to ruthenium-oxide (RuO2) there is numerous special natures, such as metallic conductivity, chemically and thermally stability, catalysis are lived
Property, electrochemical redox property and Flied emission reaction, thus all have for the research of crystallization and unformed ruthenium-oxide
Important theory and realistic meaning.In terms of electricity, oxidation ruthenium film surpasses in integrated circuit, film resistance, ferroelectric thin film and high temperature
Leading film has critically important application value.In terms of catalysis, ruthenium-oxide is active component and electricity in chlorine industry electrode
Solve water hydrogen manufacturing, photo catalytic reduction CO2With the important substance of oxidation CO sensings.In energy storage and switching device application aspect, hydroxide
Ruthenium is essential elements of the Pt-Au electrodes similar to CO poisonings for removing methanol fuel cell.Further, since itself therefore some Surface Oxygens
Change the fake capacitance of reduction ion pair and superelevation, RuO2·H2A kind of particularly important electricity of O inherently electric chemical super capacitors
Pole material.
Nanocomposite is made of two or more nano materials, due to its unique property and technique application and by
Extensive concern.Nucleocapsid and dumbbell shape structure are the most famous in nano composite structure, relative to wherein single component
Material has better optics, magnetics and catalytic performance.Do not exist at present about hud typed gold and the nano combined knot of ruthenium-oxide
The relevant report of structure is also mostly at present that ruthenium-oxide particle is deposited to gold nano for the research of gold and ruthenium-oxide composite construction
The surface of grain.
Invention content
In order to solve the above technical problems, the object of the present invention is to provide a kind of hud typed gold-ruthenium-oxide nanocomposites
And preparation method thereof, it is nano combined that hud typed gold-ruthenium-oxide has been synthesized under the conditions of high temperature hydrothermal synthesis using simple one-step method
Material, easy to operate, repetitive rate is high, and the product yield of synthesis is high, and pattern and shell thickness are easily controllable.
The present invention provides a kind of hud typed gold-ruthenium-oxide nanocomposite, gold nanoparticle including kernel and
The molar ratio of the ruthenium-oxide being coated on outside its, gold nanoparticle and ruthenium-oxide is 1:0.2-0.8.
Further, the diameter for the core that gold nanoparticle forms and oxidation in hud typed gold-ruthenium-oxide nanocomposite
The ratio between thickness of housing of ruthenium composition is 1:0.5-2.
Further, gold nanoparticle is gold nanorods, a diameter of 10-30nm, length 50-80nm.
Further, hud typed gold-ruthenium-oxide nanocomposite is in rodlike, a diameter of 20-30nm, length 60-
140nm。
Further, the UV-visible-near infrared absorption absorption peak of hud typed gold-ruthenium-oxide nanocomposite
Wavelength is between 800-1300nm.
In the present invention, gold nanoparticle is connected with each other with ruthenium-oxide by coordinate bond.Colloidal gold core is coated on oxygen
Change in ruthenium shell structurre, and shell is non-particulate for homogeneous texture, while the yield of composite material is high, pattern and shell thickness hold
It is easy to control.
The present invention also provides the preparation methods of above-mentioned hud typed gold-ruthenium-oxide nanocomposite, include the following steps：
(1) pH value of gold-containing solution is adjusted to 8-12, adds mixing after the organic solution of acetylacetone,2,4-pentanedione ruthenium, wherein institute
It states gold-containing solution and includes gold nanoparticle, quaternary cationic surfactant and water, quaternary ammonium salt is positive in gold-containing solution
A concentration of the 0.05 × 10 of ionic surface active agent-3-1.5×10-3mol/L；
(2) step (1) mixed solution at 100-120 DEG C is subjected to hydro-thermal reaction, obtains hud typed gold-ruthenium-oxide
Nanocomposite.
Further, in step (1), gold nanoparticle is gold nanorods.
Further, in step (1), the molar ratio of gold nanoparticle and quaternary cationic surfactant is 1:
0.08-2.4。
Further, in step (1), quaternary cationic surfactant for cetyl trimethylammonium bromide or
Ammonium bromide and tetraoctyl ammonium bromide.
In step (1), quaternary cationic surfactant can play the role of stabilizer, and cationic surface is lived
Property agent absorption gold nanorods surface formed bilayer gold nanorods particle is made to show electropositive, pass through electrostatic repulsion and table
Face activating agent steric hindrance maintains its stability in aqueous solution, prevents the gold nanoparticle in solution from reuniting.Rear
In continuous reaction process, gold nanoparticle becomes the nuclearing centre of acetylacetone,2,4-pentanedione ruthenium hydrolysis under the action of surfactant, raw
Into nano oxidized ruthenium shell.Nano oxidized ruthenium surface atom drops low-surface-energy on gold nanoparticle surface, forms hud typed gold-oxygen
Change ruthenium nano composite structure.After reaction, cationic surfactant present in system can prevent product it is hud typed gold-
Ruthenium-oxide nanocomposite is reunited.
The addition for adjusting cationic surfactant may be such that the pattern of final product and structure are well controlled, with
For cetyl trimethylammonium bromide (CTAB), due to gold nanoparticle adsorption Br-And Cl-Ion, gold nanoparticle
Surface gold atom be considered as with negative electrical charge.The amino with positive charge is since electrostatic interaction is by tightly in CTAB molecules
Ground is strapped in the surface of gold, forms inside points sublayer.Since hydrophobic carbochain cannot be dispersed in water, thus form another
One layer of CTAB molecular layer, the carbochain interaction that the hydrophobic carbochain of the molecular layer is inwardly directed and inside points sublayer is hydrophobic, and it is close
The head amino of water is then directed toward outside.The presence of this bilayer in gold nanoparticle surface can be determined by measuring thickness.
CTAB bilayers can destroy by the following method, as reduce solution in CTAB concentration make it below critical micelle concentration,
Add in organic solvent, the salinity in raising solution or other outside stimulus.
It is strong and weak to the attraction of nano oxidized ruthenium that gold nanoparticle surface C TAB bilayers can influence gold nanorods.Regulate and control molten
The concentration regulation and control gold nanorods surface C TAB bilayers of CTAB in liquid, regulation and control ruthenium-oxide is by dropping low-surface-energy absorption in Jenner
The complexity on rice corpuscles surface so that the pattern and structure of final product are well controlled.
Further, in step (1), the molar ratio of acetylacetone,2,4-pentanedione ruthenium and gold nanoparticle in gold-containing solution is 0.2-
0.8:1.The thickness of ruthenium-oxide shell in final product can be controlled by changing the addition of acetylacetone,2,4-pentanedione ruthenium.
Further, in step (1), a concentration of the 0.1 × 10 of acetylacetone,2,4-pentanedione ruthenium in organic solution-3-0.5×10- 3mol/L。
Further, in step (1), the organic solvent used in organic solution is methanol, ethyl alcohol, isopropanol and acetone
One or more of.
Further, in step (1), pH is adjusted using the aqueous solution of alkali, it is preferable that alkali is sodium hydroxide.
Further, it in step (2), is reacted in hydrothermal reaction kettle.
Further, in step (2), reaction time 5-30h.Preferably, reaction time 8-12h.It is highly preferred that
Reaction time is 10h.
Acetylacetone,2,4-pentanedione ruthenium hydrolyzes under the conditions of pH disclosed in this invention and reaction temperature, generates nano oxidized ruthenium,
Nano oxidized ruthenium surface atom has larger bond order missing, thus generates larger surface energy, nano oxidized ruthenium is in gold nanorods
Under attraction, surface oxidation ruthenium atom drops low-surface-energy on the surface of gold nanorods using gold atom as surface ligand, forms core
Shell mould gold-ruthenium-oxide nano composite structure.
According to the above aspect of the present invention, the present invention has at least the following advantages：
The present invention is based on the technology for hydrolyzing under acetylacetone,2,4-pentanedione ruthenium high temperature in water phase to prepare ruthenium-oxide shell structurre, the nucleocapsid
Type composite material is completed in next step in high temperature hydrothermal synthesis method, greatly reduces energy loss, more suitable for large-scale production；It closes
Into the solvent used in the process be water and a small amount of organic solvent, safe and non-toxic；Ruthenium source be the ruthenium salt containing organic matter ligand, institute
The shell of synthesis is non-particulate for homogeneous texture.This method can be generalized to similar other noble metals and oxide system, can
Using as a kind of preparation method of blanket hud typed composite material.
The preparation method of the present invention is easy to operate, and repetitive rate is high, and the product yield of synthesis is high, the pattern and shell of composite material
Layer thickness is easy to control, and the product cost synthesized is relatively low, is easy to industrialization production.
Hud typed gold-ruthenium-oxide nanocomposite prepared by method using the present invention, thermal stability significantly improve,
Compared to single gold nanoparticle, red shift occurs for the UV-visible-near infrared absorption of composite construction, and absorption peak is located at
Near infrared region has unique optics and magnetic performance, before biomedical sector and catalytic field have application well
Scape.The regulation and control method of traditional adjusting gold nanoparticle, the conjunction of high yield can be realized by structure (size and pattern) regulation and control
It is 500-900nm into gold nanorods local surface plasma resonance (LSPR) response wave length scope, near infrared region (750-
It can not 1400nm) realize the high yield synthesis of gold nano-material.Hud typed gold-ruthenium-oxide nanocomposite shows local table
The characteristic of face plasma resonance (LSPR) red shift makes hud typed gold-ruthenium-oxide nano composite structural material become a kind of and realizes height
Its local surface plasma resonance (LSPR) of the synthesis gold nano-material of yield is in the effective ways of near infrared region.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be implemented in accordance with the contents of the specification, below with presently preferred embodiments of the present invention and after attached drawing is coordinated to be described in detail such as.
Description of the drawings
Fig. 1 is the scanning electron microscope diagram piece of gold nanorods；
Fig. 2 is the scanning electron microscopy of gold nanorods/ruthenium-oxide core-shell type nano structure prepared by the embodiment of the present invention 3
Mirror picture；
Fig. 3 is gold nanorods and gold nanorods/ruthenium-oxide core-shell type nano prepared by the embodiment of the present invention 1,2 and 3
The UV-visible-near infrared absorption of structure；
Fig. 4 is the X-ray diffraction of the hud typed composite construction of gold nanorods/ruthenium-oxide prepared by the embodiment of the present invention 3
(XRD) collection of illustrative plates.
Specific embodiment
With reference to the accompanying drawings and examples, the specific embodiment of the present invention is described in further detail.Implement below
Example is used to illustrate the present invention, but be not limited to the scope of the present invention.
Embodiment 1
(1) 10 milliliters of colloidal golds stablized with cetyl trimethylammonium bromide (rodlike) are taken, with 7500 in centrifuge
Rev/min centrifugation 32 minutes, centrifugation twice, remove excessive surfactant.Then 2 ml deionized waters are added in be divided
It dissipates, the colloidal gold solution after being concentrated.
(2) colloidal gold solution after 1 milliliter of concentration is taken, adds 6.470 milliliters of water, then adds in the cetyl of 0.1mol/L
10 microlitres of trimethylammonium bromide aqueous solution, the pH value for adding sodium hydrate aqueous solution adjusting solution is 8.
(3) (acetylacetone,2,4-pentanedione ruthenium is a concentration of in methanol solution for the methanol solution of addition 0.05mL acetylacetone,2,4-pentanedione rutheniums
0.02mol/L, a concentration of the 1 × 10 of acetylacetone,2,4-pentanedione ruthenium in reaction solution-3Mol/L), reaction system keeps mixing in adition process
Uniformly.
(4) after the methanol solution of acetylacetone,2,4-pentanedione ruthenium adds in, solution is transferred in hydrothermal reaction kettle, reaction kettle is turned
It moving on in drying box, set temperature is 100 DEG C, and reaction obtains gold nanorods/ruthenium-oxide core-shell type nano structure in 10 hours or so,
Yield is 95%.
Embodiment 2
(1) 10 milliliters of colloidal golds stablized with cetyl trimethylammonium bromide (rodlike) are taken, with 7500 in centrifuge
Rev/min centrifugation 32 minutes, centrifugation twice, remove excessive surfactant.Then 2 ml deionized waters are added in be divided
It dissipates, the colloidal gold solution after being concentrated.
(2) colloidal gold solution after 1 milliliter of concentration is taken, adds 6.470 milliliters of water, then adds in the cetyl of 0.1mol/L
30 microlitres of trimethylammonium bromide aqueous solution, the pH value for adding sodium hydrate aqueous solution adjusting solution is 10.
(3) methanol solution (a concentration of 0.02mol/ of acetylacetone,2,4-pentanedione ruthenium in methanol solution of 0.1mL acetylacetone,2,4-pentanedione rutheniums is added in
L, a concentration of the 2 × 10 of acetylacetone,2,4-pentanedione ruthenium in reaction solution-3Mol/L), reaction system keeps being uniformly mixed in adition process.
(4) after the methanol solution of acetylacetone,2,4-pentanedione ruthenium adds in, solution is transferred in hydrothermal reaction kettle, reaction kettle is turned
It moving on in drying box, set temperature is 110 DEG C, and reaction obtains gold nanorods/ruthenium-oxide core-shell type nano structure in 10 hours or so,
Yield is 96%.
Embodiment 3
(1) 10 milliliters of colloidal golds stablized with cetyl trimethylammonium bromide (rodlike) are taken, with 7500 in centrifuge
Rev/min centrifugation 32 minutes, centrifugation twice, remove excessive surfactant.Then 2 ml deionized waters are added in be divided
It dissipates, the colloidal gold solution after being concentrated.
(2) colloidal gold solution after 1 milliliter of concentration is taken, adds 6.470 milliliters of water, then adds in the cetyl of 0.1mol/L
50 microlitres of trimethylammonium bromide aqueous solution, the pH value for adding sodium hydrate aqueous solution adjusting solution is 12.
(3) (acetylacetone,2,4-pentanedione ruthenium is a concentration of in methanol solution for the methanol solution of addition 0.25mL acetylacetone,2,4-pentanedione rutheniums
0.02mol/L, a concentration of the 5 × 10 of acetylacetone,2,4-pentanedione ruthenium in reaction solution-3Mol/L), reaction system keeps mixing in adition process
Uniformly.
(4) after the methanol solution of acetylacetone,2,4-pentanedione ruthenium adds in, solution is transferred in hydrothermal reaction kettle, reaction kettle is turned
It moving on in drying box, set temperature is 120 DEG C, and reaction obtains gold nanorods/ruthenium-oxide core-shell type nano structure in 10 hours or so,
Yield is 95%.
In above example of the present invention, colloidal gold used in step (1) is gold nanorods, and crystal seed method is used to prepare,
Specific preparation method is referring to document：Wu Jian, metal nanoparticle assembling and its surface phasmon enhancing optical Properties
[D], Shanghai Communications University, 2015..Fig. 1 is the scanning electron microscope diagram piece of gold nanorods.Fig. 2 is 3 institute of the embodiment of the present invention
The scanning electron microscope diagram piece of the gold nanorods of preparation/ruthenium-oxide core-shell type nano structure.Comparison diagram 1 and Fig. 2 can have found,
After reaction, gold nanorods surface has successfully coated the shell of ruthenium-oxide, between the length of 60-70nm, a diameter of 20-30nm.
Fig. 3 is gold nanorods (AuNR) and gold nanorods/ruthenium-oxide nucleocapsid prepared by the embodiment of the present invention 1,2 and 3
Type nanostructured (AuNR@RUO2) UV-visible-near infrared absorption, as can be seen from Figure in gold nanorods outer cladding
After ruthenium-oxide shell, maximum absorption band is by original 870nm or so red shift to being up to 1050nm or so, local surface etc.
Ion resonance (LSPR) prepares gold nanorods/ruthenium-oxide core-shell type nano structure and has and realize gold nano material near infrared region
Expect local surface plasma resonance (LSPR) near infrared region potentiality.
Fig. 4 is the X-ray diffraction of the hud typed composite construction of gold nanorods/ruthenium-oxide prepared by the embodiment of the present invention 3
(XRD) collection of illustrative plates.Fig. 4 gives AuNR@RuO2Nanostructured calcines the XRD spectral lines after 6h at 300 DEG C and 500 DEG C respectively.XRD
As a result AuNR@RuO are shown2Composite material shell structure is RuO2。
The above is only the preferred embodiment of the present invention, is not intended to restrict the invention, it is noted that for this skill
For the those of ordinary skill in art field, without departing from the technical principles of the invention, can also make it is several improvement and
Modification, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of hud typed gold-ruthenium-oxide nanocomposite, it is characterised in that：Gold nanoparticle and cladding including kernel
The molar ratio of ruthenium-oxide outside it, the gold nanoparticle and the ruthenium-oxide is 1:0.2-0.8.
2. hud typed gold-ruthenium-oxide nanocomposite according to claim 1, it is characterised in that：Hud typed gold-oxidation
The ratio between the diameter for the core that gold nanoparticle forms and the thickness of housing of ruthenium-oxide composition are 1 in ruthenium nanocomposite:0.5-
2。
3. hud typed gold-ruthenium-oxide nanocomposite according to claim 1, it is characterised in that：The hud typed gold-
Ruthenium-oxide nanocomposite is in rodlike, a diameter of 20-30nm, long 60-140nm.
4. the preparation method of hud typed gold-ruthenium-oxide nanocomposite described in a kind of any one of claim 1-3, special
Sign is, includes the following steps：
(1) pH value of gold-containing solution is adjusted to 8-12, adds mixing after the organic solution of acetylacetone,2,4-pentanedione ruthenium, wherein described contain
Gold solution includes gold nanoparticle, quaternary cationic surfactant and water, and quaternary ammonium salt is positive in the gold-containing solution
A concentration of the 0.05 × 10 of ionic surface active agent-3-1.5×10-3mol/L；
(2) step (1) mixed solution at 100-120 DEG C is subjected to hydro-thermal reaction, obtains the hud typed gold-ruthenium-oxide
Nanocomposite.
5. preparation method according to claim 4, it is characterised in that：In step (1), the gold nanoparticle and quaternary ammonium
The molar ratio of salt cationic surfactant is 1:0.08-2.4.
6. preparation method according to claim 4, it is characterised in that：In step (1), the quaternaries cation table
Face activating agent is cetyl trimethylammonium bromide or ammonium bromide and tetraoctyl ammonium bromide.
7. preparation method according to claim 4, it is characterised in that：In step (1), acetylacetone,2,4-pentanedione ruthenium is with described containing gold
The molar ratio of GOLD FROM PLATING SOLUTION nano-particle is 0.2-0.8:1.
8. preparation method according to claim 4, it is characterised in that：In step (1), what is used in organic solution is organic
Solvent is one or more of in methanol, ethyl alcohol, isopropanol and acetone.
9. preparation method according to claim 4, it is characterised in that：In step (2), reaction time 5-30h.
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| CN201810025853.9A CN108237223B (en) | 2018-01-11 | 2018-01-11 | Hud typed gold-ruthenium-oxide nanocomposite and preparation method thereof |
| PCT/CN2018/079280 WO2019136822A1 (en) | 2018-01-11 | 2018-03-16 | Core-shell type gold-ruthenium oxide nano-composite material and preparation method therefor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109036865A (en) * | 2018-08-01 | 2018-12-18 | 五邑大学 | Nanoporous Ag/RuO2Composite material and preparation method and application |
| CN112397316A (en) * | 2020-11-02 | 2021-02-23 | 南京信息工程大学 | Ruthenium oxide hydrate-ruthenium nanoparticle composite material and preparation method and application thereof |
| CN115196697A (en) * | 2022-08-04 | 2022-10-18 | 北京化工大学 | Transition metal doped ruthenium oxide nano material, preparation method and application thereof |
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| CN111496268A (en) * | 2020-05-13 | 2020-08-07 | 华侨大学 | Size-controllable Pt/MnO2Nano material and preparation method thereof |
| CN114411126B (en) * | 2022-01-26 | 2023-09-05 | 南雄市溢诚化工有限公司 | Activating solution based on ruthenium system and used before chemical nickel plating and preparation method thereof |
| CN117564289A (en) * | 2024-01-12 | 2024-02-20 | 中国科学技术大学 | Iridium ruthenium gold core-shell structure nano material and preparation method and application thereof |
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| CN115196697B (en) * | 2022-08-04 | 2024-02-02 | 北京化工大学 | Transition metal doped ruthenium oxide nano material, preparation method and application thereof |
Also Published As
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| WO2019136822A1 (en) | 2019-07-18 |
| CN108237223B (en) | 2019-08-06 |
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