CN109226781A - A kind of method that organic phase prepares different shape Ru nano material - Google Patents
A kind of method that organic phase prepares different shape Ru nano material Download PDFInfo
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- CN109226781A CN109226781A CN201811275704.4A CN201811275704A CN109226781A CN 109226781 A CN109226781 A CN 109226781A CN 201811275704 A CN201811275704 A CN 201811275704A CN 109226781 A CN109226781 A CN 109226781A
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- 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
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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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Abstract
The invention belongs to field of new material preparation, in particular to method that a kind of organic phase prepares different shape Ru nano material.The present invention is with RuCl3As presoma, as stabilizer and solvent, tert-butylamine borine is prepared for Ru nanocrystalline, nano wire and nanocluster using solvent-thermal method as reducing agent under inert gas protection for oleyl amine and tetrahydronaphthalene.This method simple process is efficient, reaction condition is mild, the nano material of preparation has many advantages, such as that stability is strong, is easy to modification and morphology controllable.
Description
Technical field
The invention belongs to field of new material preparation, in particular to a kind of organic phase prepares the side of different shape Ru nano material
Method.
Background technique
Nano material refers to the material for having one-dimensional size in three-dimensional dimension between 1-100nm, because nano material has
The excellent property such as big specific surface area, small-size effect and quantum size effect has become 21 century Material Field and grinds
The hot spot studied carefully.Metal nano material is even more the extensive concern for causing researcher because its is unique physico and learns property.In gold
In metal nanometer material, since noble metal nanometer material is in electronics, optics, catalysis, sensing, biomarker and photoelectric nano device
The various fields such as part have a good application prospect, thus become the emphasis researched and developed both at home and abroad.
Metal Ru nano material is with a wide range of applications in benzene hydrogenation field, simultaneously in electrolysis aquatic products hydrogen field
Show excellent catalytic performance.The catalytic performance of metal Ru and the size of Ru nano material are related to morphology.Although
It has been developed that a variety of methods for preparing Ru nano material, but all there is preparation process to varying degrees for these technologies
Ru nano material stability that is complicated, cannot adjusting, prepare simultaneously to the size and form of Ru nano material is poor, it is easy to reunite and
It is not easy the problems such as modifying.
Therefore, develop it is a kind of simple, reliable, low in cost and can at the same controllable adjustment Ru nano material size
With the new method for preparing Ru nano material of form just there is highly important theory and actual application to be worth.
Summary of the invention
To solve the above-mentioned problems, the present invention provides a kind of methods that organic phase prepares different shape Ru nano material.
It has the advantage that the Ru nano material 1. prepared morphologically in size simultaneously it is adjustable；2. the Ru nano material prepared
Stability is good, size uniformity, not easy to reunite；3. the Ru nano-material surface prepared is easy modification.
A kind of method that organic phase prepares different shape Ru nano material, which is characterized in that the Ru nanometer of this method preparation
Its form of material can be regulated and controled between nanocrystalline, nano wire and nanocluster.
The nanocrystalline size is 2.8-3.2nm.
The nanowire length is 20-40nm, diameter 2-4nm.
The nanocluster size is 80-100nm.
A kind of method that organic phase prepares different shape Ru nano material, specific preparation process are as follows:
1) taking 10-40mL volume ratio is oleyl amine: tetrahydronaphthalene=1: 1 mixed solution is added into the four diameter bottles that capacity is 150mL
In, after persistently leading to Ar gas 30min, with model MS-H-Pro+Mixing speed of the hot type magnetic stirring apparatus at 500 revs/min
The lower RuCl that 10-80mg is added3, and solution is warming up to 150-280 DEG C.
2) it is oleyl amine: tetrahydronaphthalene=1: 1 mixing that the tert-butylamine borine for weighing 9-70mg, which is dissolved in 1-6mL volume ratio,
Ultrasonic disperse is uniform in solvent.
3) mixed solution in step 2 is injected into the mixed solution of step 1), regulating step 1) in magnetic stirring apparatus
Stirring rate be 100-800 revs/min, be continually fed into Ar gas 10-60min, and keep solution in 150-280 DEG C of reaction 30-
120min。
4) by after above-mentioned solution natural cooling, addition 50-100mL volume ratio is ethyl alcohol: n-hexane=(1-5): 1 mixing
Liquid, with model MS-H-Pro+Hot type magnetic stirring apparatus under 500 revs/min of stirring rate in 60 DEG C of lasting stirrings
1min is then allowed to stand removal supernatant liquor, and above-mentioned solution is dispersed in 60mL hexane solution by this step afterwards in triplicate, just
The Ru nano material of different shape can be obtained.
The present invention has simple process, and reaction condition is mild, combined coefficient is high, is convenient for the morphology and size of nano material
Control.Have many advantages, such as that stability is strong and is easy to modify using nano material prepared by this method.
Detailed description of the invention
Fig. 1 is the nanocrystalline transmission electron microscope picture of the Ru of the preparation of the embodiment of the present invention 1.
Fig. 2 is the transmission electron microscope picture of Ru nano wire prepared by the embodiment of the present invention 2.
Fig. 3 is the transmission electron microscope picture of Ru nanocluster prepared by the embodiment of the present invention 3.
Specific embodiment
Principles and features of the present invention are described with reference to embodiments, listed give an actual example is served only for explaining this hair
It is bright, not limit the scope of the invention.
Embodiment 1
1) taking 20mL volume ratio is oleyl amine: tetrahydronaphthalene=1: 1 mixed solution is added into the four diameter bottles that capacity is 150mL,
After persistently leading to Ar gas 30min, with model MS-H-Pro+Hot type magnetic stirring apparatus under 500 revs/min of mixing speed plus
Enter the RuCl of 50mg3, uniform solution is stirred to get, then heats to 220 DEG C.
2) the tert-butylamine borine of 44mg is dissolved in 2mL volume ratio is oleyl amine: tetrahydronaphthalene=1: 1 in the mixed solvent
Ultrasonic disperse is uniform.
3) mixed solution in step 2 is injected into the mixed solution in step 1), regulating step 1) in magnetic agitation
The stirring rate of device is 100 revs/min, is continually fed into Ar gas 30min, and react 10min at 220 DEG C.
4) by after above-mentioned solution natural cooling, addition 60mL volume ratio is ethyl alcohol: n-hexane=1: 1 mixed liquor uses model
For MS-H-Pro+Hot type magnetic stirring apparatus persistently stir 1min in 60 DEG C under 500 revs/min of stirring rate, stand cold
But supernatant is outwelled afterwards, and above-mentioned solution is dispersed in 60mL hexane solution by this step afterwards in triplicate, can be obtained Ru's
It is nanocrystalline.
Embodiment 2
1) it is carried out according to embodiment 1.
2) it is carried out according to embodiment 1.
3) mixed solution in step 2 is injected into the mixed solution in step 1), adjust stirring rate be 100 turns/
Point, it is continually fed into Ar gas 30min under stiring, and react 120min at 220 DEG C.
4) it is carried out according to embodiment 1, the nano wire of Ru can be obtained.
Embodiment 3
1) it is carried out according to embodiment 1.
2) it is carried out according to embodiment 1.
3) mixed solution in step 2 is injected into the mixed solution in step 1), adjust stirring rate be 800 turns/
Point, it is continually fed into Ar gas 30min under stiring, and react 30min at 220 DEG C.
4) it is carried out according to embodiment 1, the nanocluster of Ru can be obtained.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (3)
1. a kind of method that organic phase prepares different shape Ru nano material, which is characterized in that the Ru nanometer material of this method preparation
Expect that its form can be regulated and controled between nanocrystalline, nano wire and nanocluster.
2. the method that organic phase according to claim 1 prepares different shape Ru nano material, which is characterized in that prepared
Nanocrystalline size be 2.8-3.2nm, the length of prepared nano wire is 20-40nm, diameter 2-4nm, prepared
The size of nanocluster is 80-100nm.
3. the method that organic phase according to claim 1 or 2 prepares different shape Ru nano material, preparation process include
Following step: 1. taking 10-40mL volume ratio is oleyl amine: tetrahydronaphthalene=1: it is 150mL's that 1 mixed solution, which is added into capacity,
In four diameter bottles, after persistently leading to Ar gas 30min, with model MS-H-Pro+Hot type magnetic stirring apparatus stirred at 500 revs/min
Mix the RuCl that 10-80mg is added under speed3, and solution is warming up to 150-280 DEG C；2. weighing the tert-butylamine boron of 9-70mg
It is oleyl amine that alkane, which is dissolved in 1-6mL volume ratio: tetrahydronaphthalene=1: 1 in the mixed solvent ultrasonic disperse is uniform；3. by step 2. in
Mixed solution is injected into the mixed solution of step 1., regulating step 1. in magnetic stirring apparatus stirring rate be 100-800 turn/
Point, it is continually fed into Ar gas 10-60min, and keep solution in 150-280 DEG C of reaction 30-120min；4. above-mentioned solution is naturally cold
But after, addition 50-100mL volume ratio is ethyl alcohol: n-hexane=(1-5): 1 mixed liquor, with model MS-H-Pro+Heating
Type magnetic stirring apparatus persistently stirs 1min in 60 DEG C in 500 revs/min of stirring rate, is then allowed to stand removal supernatant liquor, this step
Suddenly in triplicate after, above-mentioned solution is dispersed in 60mL hexane solution, so that it may obtain the Ru nano material of different shape.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110625136A (en) * | 2019-10-14 | 2019-12-31 | 商丘师范学院 | Method for efficiently and simply synthesizing Ru nanowire |
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| CN110625136A (en) * | 2019-10-14 | 2019-12-31 | 商丘师范学院 | Method for efficiently and simply synthesizing Ru nanowire |
| CN110625136B (en) * | 2019-10-14 | 2022-04-22 | 商丘师范学院 | Method for efficiently and simply synthesizing Ru nanowire |
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