CN108237223B - 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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- CN108237223B CN108237223B CN201810025853.9A CN201810025853A CN108237223B CN 108237223 B CN108237223 B CN 108237223B CN 201810025853 A CN201810025853 A CN 201810025853A CN 108237223 B CN108237223 B CN 108237223B
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- 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
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Abstract
The present invention relates to a kind of hud typed gold-ruthenium-oxide nanocomposites, gold nanoparticle including kernel and are coated on its external ruthenium-oxide, and 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 gold-ruthenium-oxide nanocomposite, the following steps are included: the pH value of gold-containing solution is adjusted to 8-12, it is mixed after adding the organic solution of acetylacetone,2,4-pentanedione ruthenium, wherein the gold-containing solution includes gold nanoparticle, cationic surfactant and water, and the concentration of cationic surfactant is 0.05 × 10 in the gold-containing solution‑3‑1.5×10‑3mol/L；Mixed solution is subjected to hydro-thermal reaction at 100-120 DEG C, obtains hud typed gold-ruthenium-oxide nanocomposite.Hud typed gold-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 technique
Due to ruthenium-oxide (RuO2) there is numerous special natures, as metallic conductivity, chemical and thermal 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 is super 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 the active component in chlorine industry electrode, and electricity
Solve water hydrogen manufacturing, photo catalytic reduction CO2With the important substance of oxidation CO sensing.In energy storage and switching device application aspect, hydroxide
Ruthenium is essential elements of the Pt-Au electrode similar to CO poisoning for removing methanol fuel cell.Further, since itself therefore some Surface Oxygens
Change the fake capacitance of reduction ion pair and superelevation, RuO2·H2The particularly important electricity of one kind of O inherently electric chemical super capacitor
Pole material.
Nanocomposite is made of two or more nano materials, due to its unique property and technique application and by
Extensive concern.Core-shell structure 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.
Summary of the invention
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 nanocomposites, 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 in hud typed gold-ruthenium-oxide nanocomposite and oxidation
The ratio between the thickness of shell 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, hud typed gold-ruthenium-oxide nanocomposite UV-visible-near infrared absorption absorption peak
Wavelength is between 800-1300nm.
In the present invention, gold nanoparticle and ruthenium-oxide are connected with each other 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, comprising the following steps:
(1) pH value of gold-containing solution is adjusted to 8-12, is mixed after adding the organic solution of acetylacetone,2,4-pentanedione ruthenium, wherein institute
Stating gold-containing solution includes gold nanoparticle, quaternary cationic surfactant and water, quaternary ammonium salt sun in gold-containing solution
The concentration of ionic surface active agent is 0.05 × 10-3-1.5×10-3mol/L；
(2) step (1) mixed solution is subjected at 100-120 DEG C 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 be 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 living
Property agent be adsorbed on gold nanorods surface formed bilayer so that gold nanorods particle is shown 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 under the action of surfactant, becomes the nuclearing centre of acetylacetone,2,4-pentanedione ruthenium hydrolysis, raw
At 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 the hud typed gold-of product
Ruthenium-oxide nanocomposite is reunited.
The additional amount for adjusting cationic surfactant may make the pattern of final product and structure to be 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.Amino in CTAB molecule with positive charge is since electrostatic interaction is by tightly
Ground is strapped in the surface of gold, forms inner part 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 inner part 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 bilayer can destroy by the following method, as reduce solution in CTAB concentration make it below critical micelle concentration,
Organic solvent is added, improves the salinity or other outside stimulus in solution.
It is strong and weak to the attraction of nano oxidized ruthenium that gold nanoparticle surface C TAB bilayer will affect gold nanorods.Regulate and control molten
The concentration of CTAB regulates and controls gold nanorods surface C TAB bilayer in liquid, and regulation ruthenium-oxide is adsorbed on Jenner by dropping low-surface-energy
The complexity on rice corpuscles surface, so that the pattern of final product and structure are well controlled.
Further, in step (1), the molar ratio of gold nanoparticle is 0.2- in acetylacetone,2,4-pentanedione ruthenium and gold-containing solution
0.8:1.The additional amount for changing acetylacetone,2,4-pentanedione ruthenium can control the thickness of ruthenium-oxide shell in final product.
Further, in step (1), the concentration of acetylacetone,2,4-pentanedione ruthenium is 0.1 × 10 in organic solution-3-0.5×10- 3mol/L。
Further, in step (1), 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 biggish bond order to lack, and thus generates larger surface energy, nano oxidized ruthenium is in gold nanorods
Under attraction, surface oxidation ruthenium atom drops low-surface-energy using gold atom as surface ligand on the surface of gold nanorods, 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
It is water and a small amount of organic solvent, safe and non-toxic at solvent used in process；Ruthenium source is 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 the preparation method as a kind of blanket hud typed composite material.
Preparation method of the 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
Thickness degree is easy to control, and the product cost synthesized is lower, is easy to industrialization production.
Hud typed gold-ruthenium-oxide the nanocomposite prepared using method of the invention, thermal stability are significantly improved,
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 field of biomedicine and catalytic field have application well
Scape.The regulation method of traditional adjusting gold nanoparticle, the conjunction of high yield may be implemented by structure (size and shape) regulation
It is 500-900nm, in the near infrared region (750- at gold nanorods local surface plasma resonance (LSPR) response wave length scope
It 1400nm) cannot achieve 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 realization high
Its effective ways of local surface plasma resonance (LSPR) in the near infrared region of the synthesis gold nano-material of yield.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, the following is a detailed description of the preferred embodiments of the present invention and the accompanying drawings.
Detailed description of the invention
Fig. 1 is the scanning electron microscope diagram piece of gold nanorods；
Fig. 2 is gold nanorods prepared by the embodiment of the present invention 3/ruthenium-oxide core-shell type nano structure scanning electron microscopy
Mirror picture；
Fig. 3 is gold nanorods/ruthenium-oxide core-shell type nano prepared by gold nanorods and 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) map.
Specific embodiment
With reference to the accompanying drawings and examples, specific embodiments of the present invention will be described in further detail.Implement below
Example is not intended to limit the scope of the invention for illustrating the present invention.
Embodiment 1
(1) 10 milliliters are taken with the stable colloidal gold of cetyl trimethylammonium bromide (rodlike), with 7500 in centrifuge
Rev/min centrifugation 32 minutes, centrifugation twice, remove excessive surfactant.Then 2 ml deionized waters are added to be divided
It dissipates, the colloidal gold solution after being concentrated.
(2) colloidal gold solution after taking 1 milliliter of concentration, adds 6.470 milliliters of water, and the cetyl of 0.1mol/L is then added
10 microlitres of trimethylammonium bromide aqueous solution, adding sodium hydrate aqueous solution and adjusting the pH value of solution is 8.
(3) (concentration of acetylacetone,2,4-pentanedione ruthenium is the methanol solution of addition 0.05mL acetylacetone,2,4-pentanedione ruthenium in methanol solution
0.02mol/L, the concentration of acetylacetone,2,4-pentanedione ruthenium is 1 × 10 in reaction solution-3Mol/L), reaction system keeps mixing in adition process
Uniformly.
(4) after the methanol solution of acetylacetone,2,4-pentanedione ruthenium is added, solution is transferred in hydrothermal reaction kettle, reaction kettle is turned
It moving on in drying box, setting 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 are taken with the stable colloidal gold of cetyl trimethylammonium bromide (rodlike), with 7500 in centrifuge
Rev/min centrifugation 32 minutes, centrifugation twice, remove excessive surfactant.Then 2 ml deionized waters are added to be divided
It dissipates, the colloidal gold solution after being concentrated.
(2) colloidal gold solution after taking 1 milliliter of concentration, adds 6.470 milliliters of water, and the cetyl of 0.1mol/L is then added
30 microlitres of trimethylammonium bromide aqueous solution, adding sodium hydrate aqueous solution and adjusting the pH value of solution is 10.
(3) (concentration of acetylacetone,2,4-pentanedione ruthenium is 0.02mol/ to the methanol solution of addition 0.1mL acetylacetone,2,4-pentanedione ruthenium in methanol solution
L, the concentration of acetylacetone,2,4-pentanedione ruthenium is 2 × 10 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 is added, solution is transferred in hydrothermal reaction kettle, reaction kettle is turned
It moving on in drying box, setting 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 are taken with the stable colloidal gold of cetyl trimethylammonium bromide (rodlike), with 7500 in centrifuge
Rev/min centrifugation 32 minutes, centrifugation twice, remove excessive surfactant.Then 2 ml deionized waters are added to be divided
It dissipates, the colloidal gold solution after being concentrated.
(2) colloidal gold solution after taking 1 milliliter of concentration, adds 6.470 milliliters of water, and the cetyl of 0.1mol/L is then added
50 microlitres of trimethylammonium bromide aqueous solution, adding sodium hydrate aqueous solution and adjusting the pH value of solution is 12.
(3) (concentration of acetylacetone,2,4-pentanedione ruthenium is the methanol solution of addition 0.25mL acetylacetone,2,4-pentanedione ruthenium in methanol solution
0.02mol/L, the concentration of acetylacetone,2,4-pentanedione ruthenium is 5 × 10 in reaction solution-3Mol/L), reaction system keeps mixing in adition process
Uniformly.
(4) after the methanol solution of acetylacetone,2,4-pentanedione ruthenium is added, solution is transferred in hydrothermal reaction kettle, reaction kettle is turned
It moving on in drying box, setting 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 embodiments 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, and metal nanoparticle assembling and its surface phasmon enhance 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 gold nanorods of preparation/ruthenium-oxide core-shell type nano structure scanning electron microscope diagram piece.Comparison diagram 1 and Fig. 2 can have found,
After reaction, gold nanorods surface has successfully coated the shell of ruthenium-oxide, and the length is 60-70nm, and diameter is between 20-30nm.
Fig. 3 is gold nanorods/ruthenium-oxide nucleocapsid prepared by gold nanorods (AuNR) and the embodiment of the present invention 1,2 and 3
Type nanostructure (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.
In the near infrared region, preparing gold nanorods/ruthenium-oxide core-shell type nano structure has realization gold nano material for ion resonance (LSPR)
Expect local surface plasma resonance (LSPR) potentiality in the near infrared region.
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) map.Fig. 4 gives AuNR@RuO2Nanostructure calcines the XRD spectral line after 6h at 300 DEG C and 500 DEG C respectively.XRD
AuNR@RuO as the result is shown2Composite material shell structure is RuO2。
The above is only a preferred embodiment of the present invention, it 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 (8)
1. a kind of preparation method of hud typed gold-ruthenium-oxide nanocomposite, which comprises the following steps:
(1) pH value of gold-containing solution is adjusted to 8-12, is mixed after adding the organic solution of acetylacetone,2,4-pentanedione ruthenium, wherein described contain
Gold solution includes gold nanoparticle, quaternary cationic surfactant and water, quaternary ammonium salt sun in the gold-containing solution
The concentration of ionic surface active agent is 0.05 × 10-3-1.5×10-3mol/L；
(2) step (1) mixed solution is subjected at 100-120 DEG C hydro-thermal reaction, obtains the hud typed gold-ruthenium-oxide
Nanocomposite；
Hud typed gold-ruthenium-oxide the nanocomposite includes the gold nanoparticle of kernel and the oxidation for being coated on its outside
The molar ratio of ruthenium, the gold nanoparticle and the ruthenium-oxide is 1:0.2-0.8.
2. preparation method according to claim 1, 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.
3. preparation method according to claim 1, 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.
4. preparation method according to claim 1, 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 nanoparticle is 0.2-0.8:1.
5. preparation method according to claim 1, it is characterised in that: organic used in organic solution in step (1)
Solvent is one or more of in methanol, ethyl alcohol, isopropanol and acetone.
6. preparation method according to claim 1, it is characterised in that: in step (2), reaction time 5-30h.
7. preparation method according to claim 1, it is characterised in that: golden in hud typed gold-ruthenium-oxide nanocomposite
The ratio between the thickness of shell of diameter and the ruthenium-oxide composition of the molecular core of nanoparticle is 1:0.5-2.
8. preparation method according to claim 1, it is characterised in that: the hud typed gold-ruthenium-oxide nanocomposite
In rodlike, a diameter of 20-30nm, long 60-140nm.
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| 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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| CN109036865B (en) * | 2018-08-01 | 2020-08-18 | 五邑大学 | Nanoporous Ag/RuO2Composite material and preparation method and application thereof |
| CN111496268A (en) * | 2020-05-13 | 2020-08-07 | 华侨大学 | Size-controllable Pt/MnO2Nano material and preparation method thereof |
| CN112397316B (en) * | 2020-11-02 | 2022-06-10 | 南京信息工程大学 | Ruthenium oxide hydrate-ruthenium nanoparticle composite material and preparation method and application 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 |
| 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 |
| CN117564289B (en) * | 2024-01-12 | 2024-05-17 | 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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| WO2019136822A1 (en) | 2019-07-18 |
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