CN106975756A - A kind of preparation method of rhodium tellurium alloy hollow nanotube - Google Patents
A kind of preparation method of rhodium tellurium alloy hollow nanotube Download PDFInfo
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- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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Abstract
A kind of preparation method of rhodium tellurium alloy hollow nanotube, is related to nanotube.Offer method is simple and easy to apply, can largely prepare that crystalline state is good, atom utilization is high, a kind of preparation method of rhodium tellurium alloy hollow nanotube of the high stability one-dimensional hollow nanotube-shaped material of rhodium tellurium.Prepare tellurium nano-wire；Prepare RhTe alloy nanotubes；Obtained RhTe alloy nanotubes are passed through into NaOH processing, the rhodium tellurium alloy hollow nanotube of high Rh contents is produced.Using the method for wet end chemistry, using Stability Analysis of Structures, the ultra-fine Te nano wires that can largely prepare as template is sacrificed, the RhTe hollow Nano tubulose materials of pattern rule are obtained after replacement process.Synthesis different-thickness, high aspect ratio RhTe hollow nanotubes are regulated and controled to replace reaction mechanism process by the inventory for changing the sour sodium dodecahydrate of metal precursor salt chlorine rhodium.
Description
Technical field
The present invention relates to nanotube, prepare that rhodium tellurium alloy is hollow to be received using tellurium nano-wire to sacrifice template more particularly, to one kind
The method of mitron.
Background technology
Noble metal nanometer material is widely used in catalysis, biologic medical, energy because of its unique physicochemical properties
The field such as source storage and conversion.During the past few decades, by regulating and controlling reaction thermodynamics and kinetics, the shape of noble metal nanocrystalline
Looks control synthesis has been achieved for very big progress, the noble metal nanocrystalline of various patterns is obtained in succession, but compared to palladium, platinum, gold,
For silver, because rhodium has the surface energy of superelevation, the document report on rhodium Syntheses is fewer at present.Generally believe table
Face free energy plays vital effect in crystal growing process, therefore nanocrystal is grown under thermodynamic (al) induction
The minimum pattern of total surface energy.Metal rhodium is as a kind of important catalyst, in numerous organic reaction (Halasi, G.；Bánsá
gi,T.；Solymosi, F.ChemCatChem 2009,1,311-317.) and CO catalysis oxidations (Zhang, Y.W.；Grass,
M.E.；Huang,W.Y.；Somorjai,G.Langmuir 2010,26,16463–16468.)、N0xReduce (Wang, R.；He,
H.；Wang,J.N.；Liu,L.C.；Dai, H.X.Catal.Today 2013,201,68-78.) (such as vehicle maintenance service)
Aspect has very high catalytic activity.Because rhodium is indispensable in catalyzed conversion, storage capacity is few and expensive, so how
Further improve its catalytic activity and utilization ratio be always association area important scientific problems and key technology difficulty.With receiving
The solid materials such as rice grain, nano wire, nanometer rods are compared, and hollow nano-material has low-density high-specific surface area, high atom profit
The characteristics of using efficiency；Hard template method is a kind of common effective method for preparing monodimension nanometer material, anti-especially by displacement
The mechanism pathways answered.Such as Yushan Yan seminars (Chen, Z.；Waje,M.；Li,W.；Yan,Y.Supportless Pt
and PtPd nanotubes as electrocatalysts for oxygen-reduction
Reactions.Angewandte Chemie 2007,46,4060-4063.) nano silver wire is utilized, from template is sacrificed, to prepare
Go out Pt nanotubes and PdPt alloy nanotubes, the silver-colored template that the experiment is utilized is relatively large in diameter about 40nm and due to the price valency of silver
Height, simultaneously because chlorion of the silver ion of generation easily with being introduced in reaction is reacted in displacement generates silver nitride precipitation, to final
Product is adversely affected, institute's not economic friendly in this approach.While multi-component one-dimensional nano structure is (such as：Nano wire,
Nanobelt, nanometer rods and nanotube) cooperative effect between the size of tool special construction and overlength, each component show it is excellent
Physicochemical properties and by the extensive concern of scientific circles, in catalytic process compare other nano particles for show compared with
Low dissolution rate, Oswald that moral cures and shows higher stability.What some existing document reports were synthesized with crystal seed
Method prepares nanometer framework (Xie, the S. of rhodium；Lu,N.；Xie,Z.；Wang,J.；Kim,M.J.；Xia,Y.Angewandte
Chemie 2012,51,10266-10270.) and nanocages (Xie, S.；Peng,H.C.；Lu,N.；Wang,J.；Kim,M.J.；
Xie,Z.；Xia, Y.Journal of the American Chemical Society 2013,135,16658-16667.),
But it is not related to the nanocrystalline preparation of the rhodium alloy of one-dimensional hollow structure also at present.Tellurium nano-wire due to big aspect ratio,
Less diameter, is a kind of preferable template to prepare one-dimensional noble metal nanometer material.Therefore developing one kind, operation is simple
Method come it is a large amount of prepare the high hollow nanotube-shaped material of one-dimensional rhodium tellurium of good crystalline state, high stability, atom utilization, for
Meet its following catalytic reforming, energy conversion and storage its in terms of application for be very important.For your gold improved
The service efficiency of category, strengthens its catalytic activity while the challenge that reduction usage amount is still current research is also opportunity.
The content of the invention
It is simple and easy to apply it is an object of the invention to provide method, it can largely prepare that crystalline state is good, atom utilization is high, Gao Wen
A kind of qualitatively preparation method of rhodium tellurium alloy hollow nanotube of the hollow nanotube-shaped material of one-dimensional rhodium tellurium.
The present invention's comprises the following steps that：
1) tellurium nano-wire is prepared；
2) RhTe alloy nanotubes are prepared；
3) by step 2) obtained RhTe alloy nanotubes pass through NaOH processing, and the rhodium tellurium alloy for producing high Rh contents is hollow
Nanotube.
In step 1) in, the specific method for preparing tellurium nano-wire can be：Using ascorbic acid as reducing agent, sodium tellurite
For tellurium source, hexadecyltrimethylammonium chloride is structure directing agent, prepares high-crystallinity, the tellurium nanometer of high-aspect-ratio features rule
Line.
In step 2) in, the specific method for preparing RhTe alloy nanotubes can be：With the sour sodium dodecahydrate of chlorine rhodium
For metal precursor salt, ethylene glycol is reaction dissolvent, step 1) prepare tellurium nano-wire for template and simultaneously as reducing agent,
PVP is surfactant, prepares the controllable RhTe alloy nanotubes of thickness.
The method that the present invention utilizes wet end chemistry, using Stability Analysis of Structures, the ultra-fine Te nano wires that can largely prepare as sacrificial mold
Plate, obtains the RhTe hollow Nano tubulose materials of pattern rule after replacement process.
The present invention is by changing the inventory of the sour sodium dodecahydrate of metal precursor salt chlorine rhodium to replace reaction mechanism mistake
Journey come regulate and control synthesis different-thickness, high aspect ratio RhTe hollow nanotubes.
Brief description of the drawings
Fig. 1 is the low power of the ultra-fine tellurium nano-wire prepared by the method for Green Chemistry using sodium tellurite as tellurium source
Transmission electron micrograph；
Fig. 2 is empty nanotube transmission electron micrograph in 2nm wall thickness rhodium tellurium alloys under low power；
Fig. 3 is empty nanotube transmission electron micrograph in 2nm wall thickness rhodium tellurium alloys under high power；
Fig. 4 is empty nanotube transmission electron micrograph in 3nm wall thickness rhodium tellurium alloys under low power；
Fig. 5 is empty nanotube transmission electron micrograph in 3nm wall thickness rhodium tellurium alloys under high power；
Fig. 6 is empty nanotube transmission electron micrograph in 4nm wall thickness rhodium tellurium alloys under low power；
Fig. 7 is empty nanotube transmission electron micrograph in 4nm wall thickness rhodium tellurium alloys under high power；
Fig. 8 is empty nanotube transmission electron micrograph in 5nm wall thickness rhodium tellurium alloys under low power；
Fig. 9 is empty nanotube transmission electron micrograph in 5nm wall thickness rhodium tellurium alloys under high power；
Figure 10 is empty nanotube high angle annular dark field scanning transmission electron microscope figure in RhTe；
Figure 11 is empty nanotube high angle annular dark field energy spectrum analysis linear scan figure in RhTe；
Figure 12 is empty nanotube high angle annular dark field scanning transmission electron microscope figure in RhTe；
Figure 13 is empty nanotube high angle annular dark field energy spectrum analysis Surface scan figure in RhTe.
Embodiment
Below by embodiment combination accompanying drawing, the invention will be further described.
Embodiment 1
In 50mL reactors, 1000mg ascorbic acid, 100mg cetyl trimethylammonium bromide, 40mL are added
After ultra-pure water is stirred at room temperature uniformly, 52mg sodium tellurite is added, is stirred at room temperature uniformly into milky, by 50mL inner liner of reaction kettle
It is fitted into steel bushing, is put into electric heating constant-temperature blowing drying box, is heated to 90 DEG C by 30 DEG C through 0.5h, then constant temperature 10h, it is last natural
Room temperature is cooled to, is stored in for several times with water washing with ethanol standby in ethylene glycol solution.
Product carries out systematic research through the modern nanometer test and analysis technologies of TEM to its pattern, micro-structural.
TEM (referring to Fig. 1) is characterized as ultra-fine regular Te nano thread structures, diameter 20nm or so；
Embodiment 2
The solution of 2mL embodiments 1 is taken in 50mL three-necked flasks, 19mL ethylene glycol and 200mg polyvinylpyrrolidones is added,
10min is preheated in 110 DEG C of heating stirring oil bath pan, then the scattered water of 4.7mg 12 will be dissolved in 1.25mL ethylene glycol
Close the sour sodium of chlorine rhodium to be injected into 5mL/h speed by syringe pump in preheating 10min reaction solution, injection is further continued for after terminating
1h is reacted, is stored in for several times with water washing with ethanol standby in ultra-pure water.
It is empty nanotube in thickness 2nm rhodium tellurium alloys that TEM, HRTEM, which characterize such as Fig. 2,3,.
Embodiment 3
The solution of 2mL embodiments 1 is taken in 50mL three-necked flasks, 19mL ethylene glycol and 200mg polyvinylpyrrolidones is added,
10min is preheated in 110 DEG C of heating stirring oil bath pan, then the scattered hydrations of 9.4mg 12 will be dissolved in 2.5mL ethylene glycol
Chlorine rhodium acid sodium is injected into by syringe pump with 5mL/h speed in preheating 10min reaction solution, and injection is further continued for anti-after terminating
1h is answered, is stored in for several times with water washing with ethanol standby in ultra-pure water.
It is empty nanotube in thickness 3nm rhodium tellurium alloys that TEM, HRTEM, which characterize such as Fig. 4,5,.
Embodiment 4
The solution of 2mL embodiments 1 is taken in 50mL three-necked flasks, 19mL ethylene glycol and 200mg polyvinylpyrrolidones is added,
10min is preheated in 110 DEG C of heating stirring oil bath pan, then the scattered hydrations of 18.8mg 12 will be dissolved in 5mL ethylene glycol
Chlorine rhodium acid sodium is injected into by syringe pump with 5mL/h speed in preheating 10min reaction solution, and injection is further continued for anti-after terminating
1h is answered, is stored in for several times with water washing with ethanol standby in ultra-pure water.
It is empty nanotube in thickness 4nm rhodium tellurium alloys that TEM, HRTEM, which characterize such as Fig. 6,7,.
Embodiment 5
The solution of 2mL embodiments 1 is taken in 50mL three-necked flasks, 19mL ethylene glycol and 200mg polyvinylpyrrolidones is added,
10min is preheated in 110 DEG C of heating stirring oil bath pan, then the scattered hydrations of 37.6mg 12 will be dissolved in 10mL ethylene glycol
Chlorine rhodium acid sodium is injected into by syringe pump with 5mL/h speed in preheating 10min reaction solution, and injection is further continued for anti-after terminating
1h is answered, is stored in for several times with water washing with ethanol standby in ultra-pure water.
TEM, HRTEM phenogram 8,9 is empty nanotube in different-thickness 5nm rhodium tellurium alloys.
Embodiment 6
Empty nanotube in different-thickness rhodium tellurium alloy prepared by above-described embodiment 2~5 is added 0.01-1 moles every liter
Sodium hydroxide solution in 3h processing is stirred at room temperature, empty nanotube in the rhodium tellurium alloy of high content rhodium can be prepared.This sentences reality
Example five is applied as research object
HAADF-STEM and EDX are characterized such as empty nanotube high angle annular dark field scanning transmission in Figure 10 and 11RhTe
Electron microscope picture and energy spectrum analysis linear scan figure；Such as Figure 12 and 13 energy spectrum analysis Surface scan figures；Confirm as hollow tubular
The structure of RhTe alloys.
Embodiment 7
The solution of four mL embodiments 1 is taken in 100mL three-necked flasks, 19mL ethylene glycol and 400mg polyvinylpyrrolidines is added
Ketone, 10min is preheated in 110 DEG C of heating stirring oil bath pan, then scattered 75.2mg 12 will be dissolved in 20mL ethylene glycol
The sour sodium of hydration chlorine rhodium is injected into by syringe pump with 5mL/h speed in preheating 10min reaction solution, injection terminate after followed by
Continuous reaction 1h, is stored in water washing standby in ultra-pure water for several times with ethanol.
Embodiment 8
The above-mentioned solution of 2mL is taken in 50mL three-necked flasks, 19mL ethylene glycol and 200mg polyvinylpyrrolidones is added,
10min is preheated in 80 DEG C of heating stirring oil bath pan, scattered 37.6mg 12 then will be dissolved in 10mL ethylene glycol and is hydrated chlorine
Rhodium acid sodium is injected into by syringe pump with 5mL/h speed in preheating 10min reaction solution, and injection is further continued for reaction after terminating
1h, is stored in water washing standby in ultra-pure water for several times with ethanol.
Claims (3)
1. a kind of preparation method of rhodium tellurium alloy hollow nanotube, it is characterised in that it is comprised the following steps that：
1) tellurium nano-wire is prepared；
2) RhTe alloy nanotubes are prepared；
3) by step 2) obtained RhTe alloy nanotubes pass through NaOH processing, produce the rhodium tellurium alloy hollow Nano of high Rh contents
Pipe.
2. a kind of preparation method of rhodium tellurium alloy hollow nanotube as claimed in claim 1, it is characterised in that in step 1) in, institute
State and prepare the specific method of tellurium nano-wire and be：Using ascorbic acid as reducing agent, sodium tellurite is tellurium source, cetyl trimethyl chlorine
Change ammonium is structure directing agent, prepares high-crystallinity, the tellurium nano-wire of high-aspect-ratio features rule.
3. a kind of preparation method of rhodium tellurium alloy hollow nanotube as claimed in claim 1, it is characterised in that in step 2) in, institute
State and prepare the specific methods of RhTe alloy nanotubes and be：Using the sour sodium dodecahydrate of chlorine rhodium as metal precursor salt, ethylene glycol is
Reaction dissolvent, step 1) prepare tellurium nano-wire for template and simultaneously as reducing agent, PVP is surfactant, prepares thickness
Controllable RhTe alloy nanotubes.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109453793A (en) * | 2018-10-22 | 2019-03-12 | 浙江工业大学 | A kind of overlength platinum tellurium meso-porous nano pipe elctro-catalyst and preparation method thereof |
| CN111804314A (en) * | 2020-06-09 | 2020-10-23 | 浙江工业大学 | Sugarcoated haw-shaped rhodium-tellurium nanochain catalyst for catalyzing methanol oxidation reaction and preparation method thereof |
| CN112968187A (en) * | 2021-02-02 | 2021-06-15 | 浙江工业大学 | Mesoporous rhodium hollow nanofiber electrocatalyst and preparation method thereof |
| CN113814407A (en) * | 2021-09-30 | 2021-12-21 | 华中科技大学 | Platinum-based alloy nanotube with platinum skin and preparation method and application thereof |
| CN114045519A (en) * | 2021-12-07 | 2022-02-15 | 哈尔滨工业大学（深圳） | Palladium platinum tellurium hollow cubic alloy nano catalyst and preparation method thereof |
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| CN109453793A (en) * | 2018-10-22 | 2019-03-12 | 浙江工业大学 | A kind of overlength platinum tellurium meso-porous nano pipe elctro-catalyst and preparation method thereof |
| CN111804314A (en) * | 2020-06-09 | 2020-10-23 | 浙江工业大学 | Sugarcoated haw-shaped rhodium-tellurium nanochain catalyst for catalyzing methanol oxidation reaction and preparation method thereof |
| CN112968187A (en) * | 2021-02-02 | 2021-06-15 | 浙江工业大学 | Mesoporous rhodium hollow nanofiber electrocatalyst and preparation method thereof |
| CN113814407A (en) * | 2021-09-30 | 2021-12-21 | 华中科技大学 | Platinum-based alloy nanotube with platinum skin and preparation method and application thereof |
| CN113814407B (en) * | 2021-09-30 | 2022-12-02 | 华中科技大学 | Platinum-based alloy nanotube with platinum skin and preparation method and application thereof |
| CN114045519A (en) * | 2021-12-07 | 2022-02-15 | 哈尔滨工业大学（深圳） | Palladium platinum tellurium hollow cubic alloy nano catalyst and preparation method thereof |
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