CN108326284A - A kind of Rh nano-nails cluster and its synthetic method - Google Patents
A kind of Rh nano-nails cluster and its synthetic method Download PDFInfo
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- CN108326284A CN108326284A CN201810123897.5A CN201810123897A CN108326284A CN 108326284 A CN108326284 A CN 108326284A CN 201810123897 A CN201810123897 A CN 201810123897A CN 108326284 A CN108326284 A CN 108326284A
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- 238000010189 synthetic method Methods 0.000 title claims abstract description 19
- 239000010948 rhodium Substances 0.000 claims abstract description 106
- 239000002086 nanomaterial Substances 0.000 claims abstract description 29
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 claims abstract description 24
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052703 rhodium Inorganic materials 0.000 claims abstract description 15
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 12
- -1 polyethylene Pyrrolidones Polymers 0.000 claims description 6
- 239000012046 mixed solvent Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 11
- 229920000036 polyvinylpyrrolidone Polymers 0.000 abstract description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 abstract description 9
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 abstract description 6
- 239000003054 catalyst Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 4
- 239000003381 stabilizer Substances 0.000 abstract description 4
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 abstract description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- 239000000243 solution Substances 0.000 description 15
- 239000002105 nanoparticle Substances 0.000 description 13
- 230000003647 oxidation Effects 0.000 description 9
- 238000007254 oxidation reaction Methods 0.000 description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 6
- MBVAQOHBPXKYMF-LNTINUHCSA-N (z)-4-hydroxypent-3-en-2-one;rhodium Chemical compound [Rh].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O MBVAQOHBPXKYMF-LNTINUHCSA-N 0.000 description 5
- 229920003081 Povidone K 30 Polymers 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 2
- 241000258957 Asteroidea Species 0.000 description 1
- 241001412171 Rubus corchorifolius Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical group Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- AISMNBXOJRHCIA-UHFFFAOYSA-N trimethylazanium;bromide Chemical compound Br.CN(C)C AISMNBXOJRHCIA-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/46—Ruthenium, rhodium, osmium or iridium
- B01J23/462—Ruthenium
-
- B01J35/40—
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- 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
-
- 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 belongs to the preparing technical field of inorganic nano material, a kind of rhodium nano-nail cluster and its synthetic method are specifically disclosed.This method is using acetylacetone,2,4-pentanedione rhodium as presoma, and oleyl amine and ethamine are collectively as solvent, reducing agent and pattern controlling agent, and for polyvinylpyrrolidone as stabilizer, solvent structure obtains the unique Rh nano-nails cluster of appearance structure.Rh nano-nails cluster prepared by the present invention is made of 12 Rh nano-nails, and the head of a nail of the Rh nano-nails is pentagonal pyramid, and post is pentagonal prism, and the length of single Rh nano-nails is 25~105nm, and width is 7~15nm;Prepared Rh nano-nail cluster uniform particle diameters, large specific surface area, atom utilization is high, shows good electro catalytic activity, compared with traditional Rh catalyst, electro catalytic activity significantly improves.
Description
Technical field
The invention belongs to novel nano-material and its preparing technical fields, and in particular to a kind of Rh nano-nails cluster and its synthesis
Method.
Background technology
Platinum group metal is industrial important catalyst, the high catalytic property shown in some important chemical syntheses
It can not can still substitute so far.But the natural resources of platinum group metal is more rare, expensive, higher operating costs;For this purpose,
In recent years, the nano particle for being attempted to prepare different-shape structure using nanotechnology reduces it to improve its catalytic efficiency
Dosage reduces use cost.The property of platinum group metal nano material and their particle size and appearance structure are closely related.So far
The control synthesis of the present, the accurate modulation and its pattern and surface texture of platinum group metal nano material particle size are always that nanometer is closed
At the research hotspot and challenging job of technology.Synthetic method, reducing agent type, stabilizer types, pattern controlling agent, reaction temperature
The factors such as degree, reaction pressure, reaction system pH, solvent effect can all influence the growth response dynamics mistake of metal nano material
Journey.
Rhodium is as a kind of important platinum group metal, since its own good electron transport ability is often used as a kind of typical case
Catalyst be applied among the chemical reactions such as hydrogenating reduction, cyclisation and oxidation, show high catalytic activity and catalysis selected
Selecting property.But rhodium is due to high surface free energy possessed by itself, to show higher thermodynamic phase.Therefore,
The pattern control synthesis of Rh nano particles is always one of the challenge problem in the field.Until people in 2008 are just with the tetradecane
Base trimethylammonium bromide is that stabilizer has prepared a kind of nanometer of Rh of the comparatively regular patterns-of Rh using solvent-thermal method
Cubic block.So far, the Rh nano particles of different-shape are successfully synthesized to obtain, as cube, regular octahedron, positive ten hexahedron,
The Rh nanostructures such as cube frame, recessed tetrahedron, ultrathin nanometer piece, starfish appearance, Rubus corchorifolius shape, main synthetic method are solvent heat
Method.Meanwhile people also explore these catalytic performances of Rh nano particles in thermocatalytic or photocatalysis, with the black phases of business Rh
Than catalytic activity improves a lot.But relative to other nanoparticles of platinum group metal, obtained Rh nanostructures still compared with
Lack, predominantly two dimensional surface or three-dimensional polyhedron structure;And the catalytic performance of obtained Rh nano particles still needs further
It improves.Therefore, novel Rh nanostructures and its synthetic method are further explored, there is important meaning for further increasing its performance
Justice.
Invention content
It is an object of the invention to overcome the shortcomings of that Rh appearance of nano material structure control in the prior art synthesizes, one is provided
The Rh nano materials of the new pattern of kind and its preparation method of simple and effective.
To achieve the above object, the technical solution used in the present invention is:
A kind of Rh nano-nails cluster of the present invention, is made of 12 Rh nano-nails, and the head of a nail of the Rh nano-nails is five
Pyramid, post are pentagonal prism, and the length of single nano-nail is 25~105nm, and width is 7~15nm.
The present invention also provides a kind of synthetic methods of above-mentioned Rh nano-nails cluster, specifically comprise the following steps:
(1) a certain amount of rhodium presoma and surface protectant are added in solvent and carry out mixing to obtain mixed liquor, then will
Mixed liquor is fitted into the autoclave with polytetrafluoroethyllining lining;
(2) autoclave that mixed liquor is housed in step (1) is placed in thermostatic drying chamber, and by the temperature of drying box
190~220 DEG C are risen to, then isothermal reaction certain time;
(3) cooled to room temperature after reaction, centrifuges, washs, being drying to obtain Rh nano-nail clusters.
Preferably, solvent described in step (1) is ethylamine solution and oleyl amine by volume 1:4~2:3 mixing formed
Solvent.
Preferably, the mass fraction of the ethylamine solution is 65%-70%.
Preferably, rhodium presoma described in step (1) is acetylacetone,2,4-pentanedione rhodium.
Preferably, surface protectant described in step (1) is polyvinylpyrrolidone.
Preferably, the reaction temperature in step (2) is 190~200 DEG C, and the isothermal reaction time is 8h.
Preferably, ethyl alcohol is added before centrifugation in step (3).
Compared with prior art, technique effect of the invention is:
(1) present invention has played important function using ethylamine solution and oleyl amine as mixed solvent in entire preparation system.
On the one hand, ethylamine presoma and PVP and being formed with presoma is coordinated, and controls reaction rate, and before being restored jointly with oleyl amine
Body is driven, while selective absorption is carried out in the different crystal faces of Rh nano particles, promotes the formation of Rh nano-nail clusters, to obtain shape
The uniform Rh nano-nail clusters of looks;On the other hand, since ethamine and oleyl amine mixture are as solvent, and oleyl amine is primary solvent,
Toxicity is relatively low, and reaction process is more mild, and relevant operation is completed in thermostatic drying chamber, so the influence to human body and environment
Less;In addition, PVP can prevent the reunion of metal nanoparticle mainly as dispersion stabilizer;
(2) Rh appearance of nano material of the invention is unique, and for the nano-nail cluster pattern that 12 Rh nano-nails are constituted, the head of a nail is
Pentagonal pyramid, post are pentagonal prism, uniform particle diameter, large specific surface area, atom utilization height;Meanwhile Rh nano-nails have more rib
And angle, there is more active site, and different distribution of orientations is spatially taken with 12 Rh nano-nails in cluster, thus
This kind of Rh nanostructure shows good electro catalytic activity, and compared with traditional Rh catalyst, electrocatalysis characteristic has apparent
Advantage;
(3) synthetic method of the present invention is simple and environmentally-friendly, is suitble to large-scale production.
Description of the drawings
Fig. 1 is TEM and the SEM figure that the embodiment of the present invention 1 synthesizes obtained Rh nano-nail clusters;
Fig. 2 is TEM and the SEM figure that the embodiment of the present invention 2 synthesizes obtained Rh nano-nail clusters;
Fig. 3 is TEM and the SEM figure that the embodiment of the present invention 3 synthesizes obtained Rh nano-nail clusters;
Fig. 4 is TEM and the SEM figure that the embodiment of the present invention 4 synthesizes obtained Rh nano-nail clusters;
Fig. 5 is TEM and the SEM figure that the embodiment of the present invention 5 synthesizes obtained Rh nano-nail clusters;
Fig. 6 is the XRD diffracting spectrums for the Rh nano-nail clusters that the embodiment of the present invention 1 synthesizes;
Fig. 7 is that the electro-catalysis methanol oxidation for the Rh nano-nail clusters that the embodiment of the present invention 1 synthesizes and the electricity of Rh nano particles are urged
Change performance and compares figure;
Fig. 8 is the TEM figures of Rh nano particles described in the embodiment of the present invention 1.
Specific implementation mode
Technical scheme of the present invention is further elaborated with reference to embodiment:
Embodiment 1
A kind of synthetic method of Rh nano materials, includes the following steps:
A, by 10mg acetylacetone,2,4-pentanediones rhodium (Rh (acac)3) and 111.1mg polyvinylpyrrolidones (PVP-K30) be dissolved in
The in the mixed solvent of the ethylamine solution and 4mL oleyl amines of 1mL 70wt% obtains mixed liquor, is packed into the high pressure with polytetrafluoroethyllining lining
In reaction kettle;
B, the autoclave equipped with mixed liquor is placed in thermostatic drying chamber, temperature is from room temperature to 200 DEG C, then
Keep isothermal reaction 8h;
C, stop reaction, cooled to room temperature obtains the colloidal solution of celadon, the second of 4 times of its volume is added later
Alcohol, centrifugal purification wash repeatedly 5 times, and Rh nano materials are obtained after dry.It is in nano-nail by Rh nano materials manufactured in the present embodiment
Cluster pattern, each nano-nail cluster are made of 12 Rh nano-nails, and the head of a nail of the Rh nano-nails is pentagonal pyramid, and post is five ribs
Column, single Rh nano-nails length about 45nm, width is about 8nm, sees Fig. 1.
XRD characterization is carried out to the Rh nano-nail clusters that embodiment 1 synthesizes, as a result shows that Rh nano-nail clusters are face-centred cubic structure
(see attached drawing 6).
The Rh nano materials synthesized using embodiment 1 test its electrocatalytic oxidation property to methanol as catalyst.Respectively will
Rh nano-nails cluster and Rh are nano-particle modified on glass-carbon electrode.Using the glass-carbon electrode of Rh modifications as working electrode, it is saturated calomel
Electrode is reference electrode, and platinum electrode is to electrode, in 0.1molL-1HClO4And 0.2molL-1CH3In OH mixed solutions-
With 50mVs between 0.2~1.2V-1Sweep speed test loop volt-ampere curve investigates electro-catalysis of the Rh nano-nails cluster to methanol
Oxidation susceptibility, and compareed with Rh nano particles.
The result shows that Rh nano-nail clusters prepared by embodiment 1 have good electro catalytic activity, Electrocatalytic Oxidation of Methanol
Oxidation peak current density is 1.64mAcm-2, and the oxidation peak current density of Rh nano particle Electrocatalytic Oxidation of Methanol is
0.53mA·cm-2, Rh nano-nail clusters are in HClO4The catalytic activity of Oxidation of Methanol is 3.1 times of Rh nano particles (see attached in solution
Fig. 7).
Embodiment 2
A kind of synthetic method of Rh nano materials, includes the following steps:
A, by 10mg acetylacetone,2,4-pentanediones rhodium (Rh (acac)3) and 111.1mg polyvinylpyrrolidones (PVP-K30) be dissolved in
Then mixed liquor is packed into polytetrafluoroethyllining lining by the ethylamine solution of 2mL 70wt% with the mixed solution of 3mL oleyl amines
In autoclave;
B, the autoclave equipped with mixed liquor is placed in thermostatic drying chamber, temperature is from room temperature to 200 DEG C, then
Keep isothermal reaction 8h;
C, stop reaction, cooled to room temperature obtains the colloidal solution of celadon, the second of 4 times of its volume is added later
Alcohol centrifugal purification, washing obtain the Rh nano materials in nano-nail cluster pattern after dry.By Rh nano materials manufactured in the present embodiment
In nano-nail cluster pattern, each nano-nail cluster is made of 12 Rh nano-nails, and the head of a nail of the Rh nano-nails is pentagonal pyramid, post
For pentagonal prism, single Rh nano-nails length about 90nm, post width is about 14nm, sees Fig. 2.
Embodiment 3
A kind of synthetic method of Rh nano materials, steps are as follows:
A, by 10mg acetylacetone,2,4-pentanediones rhodium (Rh (acac)3) and 111.1mg polyvinylpyrrolidones (PVP-K30) be dissolved in
The ethylamine solution of 1mL 70wt% is fitted into the mixed solution of 4mL oleyl amines in the autoclave with polytetrafluoroethyllining lining;
B, the autoclave equipped with mixed liquor is placed in thermostatic drying chamber, temperature is from room temperature to 200 DEG C, then
Keep isothermal reaction 4h;
C, stop reaction, cooled to room temperature obtains the colloidal solution of celadon, the second of 4 times of its volume is added later
Alcohol centrifugal purification, cleaning obtain the Rh nano materials in nano-nail cluster pattern after dry.By Rh nano materials manufactured in the present embodiment
In nano-nail cluster pattern, each nano-nail cluster is made of 12 Rh nano-nails, and the head of a nail of the Rh nano-nails is pentagonal pyramid, post
For pentagonal prism, single Rh nano-nails length about 28nm, width is about 9nm, sees Fig. 3.
Embodiment 4
A kind of synthetic method of Rh nano materials, steps are as follows:
A, by 10mg acetylacetone,2,4-pentanediones rhodium (Rh (acac)3) and 111.1mg polyvinylpyrrolidones (PVP-K30) be dissolved in
The ethylamine solution of 1mL 70wt% is fitted into the mixed solution of 4mL oleyl amines in the autoclave with polytetrafluoroethyllining lining;
B, the autoclave equipped with mixed liquor is placed in thermostatic drying chamber, temperature is from room temperature to 190 DEG C, then
Keep isothermal reaction 8h;
C, stop reaction, cooled to room temperature obtains the colloidal solution of celadon, the second of 4 times of its volume is added later
Alcohol centrifugal purification, cleaning obtain Rh nano materials after dry.It is in nano-nail cluster pattern by Rh nano materials manufactured in the present embodiment,
Each nano-nail cluster is made of 12 Rh nano-nails, and the head of a nail of the Rh nano-nails is pentagonal pyramid, and post is pentagonal prism, single
Rh nano-nails length about 35nm, width is about 8nm, sees Fig. 4.
Embodiment 5
A kind of synthetic method of Rh nano materials, steps are as follows:
A, by 10mg acetylacetone,2,4-pentanediones rhodium (Rh (acac)3) and 55.6mg polyvinylpyrrolidones (PVP-K30) be dissolved in 1mL
The ethylamine solution of 70wt% is fitted into the mixed solution of 4mL oleyl amines in the autoclave with polytetrafluoroethyllining lining;
B, the autoclave equipped with mixed liquor is placed in thermostatic drying chamber, temperature is from room temperature to 200 DEG C, then
Keep isothermal reaction 8h;
C, stop reaction, cooled to room temperature obtains the colloidal solution of celadon, the second of 4 times of its volume is added later
Alcohol centrifugal purification, cleaning obtain Rh nano materials after dry.It is in nano-nail cluster pattern by Rh nano materials manufactured in the present embodiment,
Each nano-nail cluster is made of 12 Rh nano-nails, and the head of a nail of the Rh nano-nails is pentagonal pyramid, and post is pentagonal prism, single
Rh nano-nails length about 31nm, width is about 8nm, sees Fig. 5.
Finally it should be noted that:The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention.
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
With technical scheme described in the above embodiments is modified or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in the present invention's
Within protection domain.
Claims (7)
1. a kind of Rh nano-nails cluster, which is characterized in that the Rh nano-nails cluster is made of 12 Rh nano-nails, the nano-nail
The head of a nail is pentagonal pyramid, and post is pentagonal prism, and the length of single nano-nail is 25~105nm, and width is 7~15nm.
2. the synthetic method of Rh nano-nails cluster described in a kind of claim 1, which is characterized in that include the following steps:
(1) a certain amount of rhodium presoma, surface protectant are added in solvent and carry out mixing to obtain mixed liquor, then by mixed liquor
It is fitted into the autoclave with polytetrafluoroethyllining lining;
(2) autoclave that mixed liquor is housed in step (1) is placed in thermostatic drying chamber, and the temperature of drying box is risen to
190~220 DEG C, then isothermal reaction certain time;
(3) cooled to room temperature after reaction, centrifuges, washs, being drying to obtain Rh nano materials.
3. synthetic method according to claim 2, which is characterized in that solvent described in step (1) is ethylamine solution and oil
Amine by volume 1:4~2:3 mixed solvents formed.
4. synthetic method according to claim 2, which is characterized in that rhodium presoma described in step (1) is acetylacetone,2,4-pentanedione
Rhodium.
5. synthetic method according to claim 2, which is characterized in that surface protectant described in step (1) is polyethylene
Pyrrolidones.
6. synthetic method according to claim 2, which is characterized in that the reaction temperature in step (2) is about 190~200
DEG C, the isothermal reaction time is 8h.
7. synthetic method according to claim 3, which is characterized in that the mass fraction of the ethylamine solution is 65%-
70%.
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CN109078634A (en) * | 2018-08-22 | 2018-12-25 | 国家纳米科学中心 | A kind of Pt/Rh nanocomposite and its preparation method and application |
CN109226781A (en) * | 2018-10-30 | 2019-01-18 | 郑州大学 | A kind of method that organic phase prepares different shape Ru nano material |
CN111266600A (en) * | 2020-03-18 | 2020-06-12 | 陕西师范大学 | Efficient preparation method of multilevel spherical rhodium nanocrystals |
CN111438372A (en) * | 2020-05-12 | 2020-07-24 | 中南民族大学 | Coralline Rh nano-particles and synthesis method thereof |
CN111496267A (en) * | 2020-05-12 | 2020-08-07 | 中南民族大学 | Folding Rh nanosheet and synthesis method thereof |
Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1299720A (en) * | 1999-12-13 | 2001-06-20 | 中国科学院化学研究所 | Preparation of nanometer-level platinum metal cluster |
US7767610B1 (en) * | 2004-02-25 | 2010-08-03 | Sandia Corporation | Metal nanoparticles as a conductive catalyst |
CN102553579A (en) * | 2011-05-27 | 2012-07-11 | 中国科学院福建物质结构研究所 | Preparation method of high-dispersity supported nano metal catalyst |
CN102863012A (en) * | 2012-09-26 | 2013-01-09 | 深圳大学 | Synthetic method of zinc oxide nanometer nail |
CN103397387A (en) * | 2013-07-05 | 2013-11-20 | 浙江大学 | Preparation method of rhodium-palladium alloy nano dendrite and rhodium-palladium alloy nano dendrite prepared by same |
CN103658673A (en) * | 2013-11-27 | 2014-03-26 | 浙江大学 | Preparation method and products of rhodium-palladium alloy nanocrystal |
CN103696000A (en) * | 2013-11-27 | 2014-04-02 | 浙江大学 | Rhodium nanocrystal and preparation method thereof |
CN104549244A (en) * | 2015-02-06 | 2015-04-29 | 厦门大学 | Rhodium nanometer catalyst as well as preparation method and application thereof |
CN106112009A (en) * | 2016-08-24 | 2016-11-16 | 浙江大学 | A kind of rhodio-platinum alloy nano flower and preparation method thereof |
CN106493386A (en) * | 2016-11-03 | 2017-03-15 | 国家纳米科学中心 | The octahedral shape Nanoalloy of octahedra Nanoalloy and porous, Preparation Method And The Use |
-
2018
- 2018-02-07 CN CN201810123897.5A patent/CN108326284B/en active Active
Patent Citations (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1299720A (en) * | 1999-12-13 | 2001-06-20 | 中国科学院化学研究所 | Preparation of nanometer-level platinum metal cluster |
US7767610B1 (en) * | 2004-02-25 | 2010-08-03 | Sandia Corporation | Metal nanoparticles as a conductive catalyst |
CN102553579A (en) * | 2011-05-27 | 2012-07-11 | 中国科学院福建物质结构研究所 | Preparation method of high-dispersity supported nano metal catalyst |
CN102863012A (en) * | 2012-09-26 | 2013-01-09 | 深圳大学 | Synthetic method of zinc oxide nanometer nail |
CN102863012B (en) * | 2012-09-26 | 2014-12-03 | 深圳大学 | Synthetic method of zinc oxide nanometer nail |
CN103397387A (en) * | 2013-07-05 | 2013-11-20 | 浙江大学 | Preparation method of rhodium-palladium alloy nano dendrite and rhodium-palladium alloy nano dendrite prepared by same |
CN103658673A (en) * | 2013-11-27 | 2014-03-26 | 浙江大学 | Preparation method and products of rhodium-palladium alloy nanocrystal |
CN103696000A (en) * | 2013-11-27 | 2014-04-02 | 浙江大学 | Rhodium nanocrystal and preparation method thereof |
CN104549244A (en) * | 2015-02-06 | 2015-04-29 | 厦门大学 | Rhodium nanometer catalyst as well as preparation method and application thereof |
CN106112009A (en) * | 2016-08-24 | 2016-11-16 | 浙江大学 | A kind of rhodio-platinum alloy nano flower and preparation method thereof |
CN106493386A (en) * | 2016-11-03 | 2017-03-15 | 国家纳米科学中心 | The octahedral shape Nanoalloy of octahedra Nanoalloy and porous, Preparation Method And The Use |
Cited By (7)
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CN109078634A (en) * | 2018-08-22 | 2018-12-25 | 国家纳米科学中心 | A kind of Pt/Rh nanocomposite and its preparation method and application |
CN109226781A (en) * | 2018-10-30 | 2019-01-18 | 郑州大学 | A kind of method that organic phase prepares different shape Ru nano material |
CN111266600A (en) * | 2020-03-18 | 2020-06-12 | 陕西师范大学 | Efficient preparation method of multilevel spherical rhodium nanocrystals |
CN111438372A (en) * | 2020-05-12 | 2020-07-24 | 中南民族大学 | Coralline Rh nano-particles and synthesis method thereof |
CN111496267A (en) * | 2020-05-12 | 2020-08-07 | 中南民族大学 | Folding Rh nanosheet and synthesis method thereof |
CN111496267B (en) * | 2020-05-12 | 2022-05-13 | 中南民族大学 | Folding Rh nanosheet and synthesis method thereof |
CN111438372B (en) * | 2020-05-12 | 2022-08-05 | 中南民族大学 | Coral-shaped Rh nano-particles and synthesis method thereof |
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