CN109926575A - A kind of copper method for preparing Nano cube - Google Patents
A kind of copper method for preparing Nano cube Download PDFInfo
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- CN109926575A CN109926575A CN201711355851.8A CN201711355851A CN109926575A CN 109926575 A CN109926575 A CN 109926575A CN 201711355851 A CN201711355851 A CN 201711355851A CN 109926575 A CN109926575 A CN 109926575A
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- copper
- ethylene glycol
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Abstract
The present invention relates to a kind of copper method for preparing Nano cube, and the copper nanocube of different side lengths is prepared using seed mediated growth method.It uses ethylene glycol first as solvent and reducing agent, PVP is stabilizer, trifluoracetic acid copper is that copper source, hydrochloric acid and soluble sulphurizing salt are the copper cube seed that adjuvant prepares that average side length is 35 nm；Then ethylene glycol is used as solvent and reducing agent, PVP are stabilizer and soluble copper salt is copper source, by controlling the relative usage of seed and mantoquita, has obtained the copper nanocube that average side length is 40-160 nm.The method of the present invention is easy to operate, process control, obtained copper nanocube stability are high, is a kind of method for efficiently synthesizing copper nanocube, therefore have a vast market foreground.
Description
Technical field
The present invention relates to nano-functional material technical fields, and in particular to a kind of copper method for preparing Nano cube.
Background technique
Copper nano material has unique optical property, electrical properties, catalytic property and excellent sensing capability and life
Analyte detection ability, therefore the copper nano material of various patterns receives extensive research.Compared to spherical shape, grain of rice type, rodlike, band
The copper nano-particle of the patterns such as shape, threadiness, cubic type is of greatest concern.Copper nanocube corner angle are sharp, pattern is uniform, can be with
As highly sensitive local plasmon sensing and surface enhanced Raman substrate.And copper nanocube can be used as sacrifice template
Cubic type structure, such as Cu, Pb, Pt and Au etc. for synthesizing various metals.
Currently, being developed a variety of methods for preparing copper nanocube, there are polyhydroxy reduction method, hydrothermal synthesis
Method, using octahedral figure gold particle as epitaxial growth method of seed etc..Tao etc. using 1,5-PD as reducing agent and solvent,
PVP is stabilizer and copper nitrate is copper source, by polyhydroxy reduction method obtained side length be 80 nm copper cube (Tao,
A.;Sinsermsuksakul, P. and Yang, P. D. Angew. Chem. 2006,118,4713-4717).
Chen etc. is prepared for the copper nanocube that side length is 58 nm using high temperature hydrothermal method.This method uses poly dimethyl diene
Propyl ammonium chloride is stabilizer and reducing agent, and copper nitrate is copper source, in 170 DEG C of 16 h(Inorg. Chem. of hydro-thermal reaction
2007,46,10587-10593).
But all there are some disadvantages in these methods, for example the reaction time is long, size controlling is inhomogenous, low yield and repetition
Property is poor.Therefore the method for exploitation high efficiency and high quality synthesis copper nanocube is still the emphasis of research.
Summary of the invention
The technical problem to be solved in the present invention is to provide the copper nanometers for preparing of a kind of high efficiency, high yield and high duplication to stand
The method of cube.
In order to solve the above technical problems, the technical scheme is that step 1: using ethylene glycol as solvent and reducing agent,
Trifluoracetic acid copper is copper source, PVP is that stabilizer, hydrochloric acid and soluble sulphurizing salt are adjuvant, is made using polyhydroxy reduction method
Average side length is the copper cube seed of 35 nm；
Step 2: being solvent and reducing agent, PVP as stabilizer, soluble copper salt using ethylene glycol
For copper source, the copper cube seed that a certain amount of side length is 35 nm is added, use seed mediated growth method be made average side length for
The copper nanocube of 40-160nm.
The specific steps of the preparation method are as follows:
Step 1: 5mL ethylene glycol is added first in the three-necked flask of 50mL, with oil bath heating to 150 DEG C, and temperature is permanent
Be scheduled on 150 DEG C, then sequentially add 0.06 mL 3mM sulphurizing salt ethylene glycol solution, 0.5mL 3mM HCl ethylene glycol solution,
200 mM trifluoracetic acid copper ethylene glycol solution of 1.25mL 20mg/mL PVP ethylene glycol solution and 0.4mL；Use ultravioletvisible absorption
Flask is taken out when ultraviolet absorption peak appears near 350nm and 435nm and immerses ice by the degree that spectrum monitoring reaction carries out
Water-bath is reacted to terminate, and obtained copper nanocube seed average side length is 35 nm, is washed repeatedly with second alcohol and water repeatedly
Afterwards, it is dispersed in water preservation, the concentration of copper seed is 9 × 1020A/mL；
Step 2: 1.25 mL ethylene glycol are added in the beaker of 10mL, with oil bath heating to 150 DEG C, 0.3mL is then added
20mg/mL PVP ethylene glycol solution, and the copper nano cubic that 10-200 μ L average side length is 35nm is added by certain volume ratio
The ethylene glycol solution of body seed and 10-200 μ L 200mM mantoquita reacts to take out flask after carrying out 3 h and immerses ice-water bath eventually
It only reacts, after obtained copper nanocube second alcohol and water washs repeatedly repeatedly, is dispersed in water preservation.
The molecular weight of above-mentioned PVP is 5500.
Above-mentioned sulphurizing salt is one of vulcanized sodium, NaHS, potassium sulfide.
Above-mentioned mantoquita is one of copper nitrate and trifluoracetic acid copper.
The volume ratio for the copper cube seed that the ethylene glycol solution and side length of the mantoquita are 35nm is 0.1-10:1.
The copper nanocube that the present invention is prepared, partial size is uniform in monodispersity, pattern, grows mantoquita by adjusting
Can have high duplication and high yield with the relative usage of copper seed with the side length of accuracy controlling particle, this method, be a kind of high
The method of effect preparation high-quality copper nanocube, has a vast market foreground.
Specific embodiment
The present invention will be further described in detail with reference to the specific embodiments.
Embodiment 1:
Step 1: by 5mL ethylene glycol be added 50mL three-necked flask in, with oil bath heating to 150 DEG C, and by temperature it is constant
150 DEG C, then sequentially add 0.06mL 3mM NaHS ethylene glycol solution, 0.5mL 3mMHCl ethylene glycol solution, 1.25mL
20mg/mL PVP ethylene glycol solution and 0.4mL 200mM trifluoracetic acid copper ethylene glycol solution.It is supervised with ultraviolet-visible absorption spectroscopy
The degree that reaction carries out is surveyed, when ultraviolet and visible absorption peak appears near 350 nm and 435 nm, flask is taken out and immerses ice
After being centrifuged repeatedly washing repeatedly with second alcohol and water, nanometer seeded dispersion is saved in water with terminating reaction for water-bath, copper seed
Concentration is 9 × 1020A/mL, average side length are 35 nm；
Step 2: 1.25mL ethylene glycol is added in the beaker of 10mL, with oil bath heating to 150 DEG C, 0.3mL is then added
The average side length of 20mg/mL PVP ethylene glycol solution, the preparation of the 200 μ L first steps is the copper nanocube seed and 20 of 35 nm
Flask taking-up immersion ice-water bath is reacted to terminate after carrying out 3 h, is put down by the ethylene glycol solution of μ L 200mM copper nitrate, reaction
After the copper nanocube second alcohol and water that equal side length is 40 nm washs repeatedly repeatedly, it is dispersed in water preservation.
Embodiment 2:
1.25mL ethylene glycol is added in the beaker of 10mL, with oil bath heating to 150 DEG C.Then 0.3 mL 20mg/mL is added
The average side length of PVP ethylene glycol solution, the preparation of 100 μ L embodiment, 1 first step is the copper nanocube seed and 100 μ of 35 nm
Flask taking-up immersion ice-water bath is reacted to terminate after carrying out 3 h, is put down by the ethylene glycol solution of L 200mM copper nitrate, reaction
After the copper nanocube second alcohol and water that equal side length is 56 nm washs repeatedly repeatedly, it is dispersed in water preservation.
Embodiment 3:
Step 1: by 5mL ethylene glycol be added 50mL three-necked flask in, with oil bath heating to 150 DEG C, and by temperature it is constant
150 ℃.Then sequentially add 0.06mL 3mM potassium sulfide ethylene glycol solution, 3 mM HCl ethylene glycol solution of 0.5mL,
1.25mL 20mg/mL PVP ethylene glycol solution and 0.4mL 200mM trifluoracetic acid copper ethylene glycol solution, are inhaled with UV, visible light
The degree that spectrum monitoring reaction carries out is received to take flask when ultraviolet and visible absorption peak appears near 350 nm and 435 nm
It immerses ice-water bath out to terminate reaction, after being centrifuged repeatedly washing repeatedly with second alcohol and water, nanometer seeded dispersion is saved in water,
The concentration of copper seed is 9 х 1020A/mL, average side length are 35 nm；
Step 2: 1.25mL ethylene glycol is added in the beaker of 10mL, with oil bath heating to 150 DEG C, 0.3mL 20 is then added
The average side length of mg/mL PVP ethylene glycol solution, the preparation of the 200 μ L first steps is the copper nanocube seed and 50 μ L of 35nm
The ethylene glycol solution of 200mM trifluoracetic acid copper.Reaction reacts flask taking-up immersion ice-water bath to terminate after carrying out 3 h, obtains
Average side length is after the copper nanocube second alcohol and water of 94 nm washs repeatedly repeatedly, to be dispersed in water preservation.
Embodiment 4:
1.25mL ethylene glycol is added in the beaker of 10mL, with oil bath heating to 150 DEG C, 0.3 mL, 20 mg/ is then added
ML PVP ethylene glycol solution, 200 μ L embodiment, 3 first step preparation average side length be 35 nm copper nanocube seed and
The ethylene glycol solution of 20 μ L 200mM trifluoracetic acid coppers, reaction react flask taking-up immersion ice-water bath to terminate after carrying out 3 h,
Obtain the copper nanocube second alcohol and water that average side length is 148 nm wash repeatedly it is multiple after, be dispersed in water preservation.
Claims (6)
1. a kind of copper method for preparing Nano cube, it is characterised in that the following steps are included::
Step 1: using ethylene glycol be solvent and reducing agent, trifluoracetic acid copper as copper source, PVP be stabilizer, hydrochloric acid and soluble sulphur
Salt dissolving is adjuvant, uses polyhydroxy reduction method that average side length is made as the copper cube seed of 35 nm；
Step 2: being solvent using ethylene glycol and reducing agent, PVP are stabilizer, soluble copper salt for copper source, a certain amount of side is added
The copper cube seed of a length of 35 nm, the copper nanocube for using seed mediated growth method that average side length is made as 40-160nm.
2. copper method for preparing Nano cube according to claim 1, it is characterised in that: the preparation method it is specific
Step are as follows:
Step 1: 5mL ethylene glycol is added first in the three-necked flask of 50mL, with oil bath heating to 150 DEG C, and temperature is permanent
Be scheduled on 150 DEG C, then sequentially add 0.06 mL 3mM sulphurizing salt ethylene glycol solution, 0.5mL 3mM HCl ethylene glycol solution,
200 mM Silver Trifluoroacetate ethylene glycol solution of 1.25mL 20mg/mL PVP ethylene glycol solution and 0.4mL；Use ultravioletvisible absorption
Flask is taken out when ultraviolet absorption peak appears near 350nm and 435nm and immerses ice by the degree that spectrum monitoring reaction carries out
Water-bath is reacted to terminate, and obtained copper nanocube seed average side length is 35 nm, is washed repeatedly with second alcohol and water repeatedly
Afterwards, it is dispersed in water preservation, the concentration of copper seed is 9 × 1020A/mL；
Step 2: 1.25 mL ethylene glycol are added in the beaker of 10mL, with oil bath heating to 150 DEG C, 0.3mL is then added
20mg/mL PVP ethylene glycol solution, and the copper nano cubic that 10-200 μ L average side length is 35nm is added by certain volume ratio
The ethylene glycol solution of body seed and 10-200 μ L 200mM mantoquita reacts to take out flask after carrying out 3 h and immerses ice-water bath eventually
It only reacts, after obtained copper nanocube second alcohol and water washs repeatedly repeatedly, is dispersed in water preservation.
3. copper method for preparing Nano cube according to claim 1 or 2, it is characterised in that: the molecular weight of the PVP
It is 5500.
4. copper method for preparing Nano cube according to claim 1 or 2, it is characterised in that: the sulphurizing salt is sulphur
Change one of sodium, NaHS, potassium sulfide.
5. copper method for preparing Nano cube according to claim 1 or 2, it is characterised in that: the silver salt is nitric acid
One of copper and trifluoracetic acid copper.
6. copper method for preparing Nano cube according to claim 2, it is characterised in that: the ethylene glycol of the mantoquita is molten
The volume ratio for the copper cube seed that liquid and side length are 35nm is 0.1-10:1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112296347A (en) * | 2019-07-29 | 2021-02-02 | 本田技研工业株式会社 | Method for preparing copper nanocubes by using tributylphosphine as ligand |
| CN114951682A (en) * | 2022-05-27 | 2022-08-30 | 郑州大学 | Method for preparing Cu nano square through crystal face regulation and control and application thereof |
-
2017
- 2017-12-16 CN CN201711355851.8A patent/CN109926575A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112296347A (en) * | 2019-07-29 | 2021-02-02 | 本田技研工业株式会社 | Method for preparing copper nanocubes by using tributylphosphine as ligand |
| CN112296347B (en) * | 2019-07-29 | 2023-04-18 | 本田技研工业株式会社 | Method for preparing copper nanocubes by using tributylphosphine as ligand |
| CN114951682A (en) * | 2022-05-27 | 2022-08-30 | 郑州大学 | Method for preparing Cu nano square through crystal face regulation and control and application thereof |
| CN114951682B (en) * | 2022-05-27 | 2023-06-27 | 郑州大学 | Method for preparing Cu nano square by crystal face regulation and control and application thereof |
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