CN108127125A - A kind of preparation method of the copper nanometer sheet of high stability - Google Patents
A kind of preparation method of the copper nanometer sheet of high stability Download PDFInfo
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- CN108127125A CN108127125A CN201611091728.5A CN201611091728A CN108127125A CN 108127125 A CN108127125 A CN 108127125A CN 201611091728 A CN201611091728 A CN 201611091728A CN 108127125 A CN108127125 A CN 108127125A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The present invention provides a kind of preparation method of the copper nanometer sheet of high stability, and alkyl trimethyl quaternary ammonium salt type surfactant and copper ion salt are dissolved in water hybrid reaction by this method, then through reduction reaction, after isolating and purifying, the copper nanometer sheet of high stability is made.This method is easy to operate, time-consuming short, and without large-scale instrument and the reaction condition of harshness, the copper nanometer sheet of different fluorescent emission intensities is can obtain by adjusting alkyl trimethyl quaternary ammonium salt, copper ion salt, reducing agent ratio.The copper nanometer tablet stability that this method obtains is good, and fluorescence efficiency is high, is prepared in photoelectric device, and sensing detection etc. has potential application value.
Description
Technical field
The invention belongs to metal nano material fields, and in particular to a kind of preparation method of the copper nanometer sheet of high stability.
Background technology
Broadly metal nano material refers at least one-dimensional in nano-scale range (1-100nm) or by this in three-dimensional system
A little basic units are formed.Nano material is since with catalytic activity height, absorbing ability is high, and mouldability is good, and hardness is high, conductivity
Greatly, the advantages that high diffusibility, high specific heat so that it has greatly application in optics, electricity, catalysis, magnetic Nano material
Value.
Since copper is relatively abundant in nature resource, and copper nano material has and gold, silver nanometer in optics, electricity etc.
The similar superior function of material, causes extensive concern in the latest 20 years.Compared to gold, silver nano material, although copper is certainly
Right boundary is resourceful, cheaper, but stability is poor.At present there are many copper nano material synthetic method, including hydro-thermal
Synthetic method, gas evaporation method, sol-gel method, laser ablation, electrochemical method etc..Wherein, it is organic with water soluble polymer
Object or surfactant synthesize copper nano material as ligand, can not use organic solvent and reduce environmental pollution, thus receive
Concern.But the copper nano material that these methods obtain is due to easily being aoxidized, there are stability it is poor the shortcomings that, the copper nanometer material of synthesis
Material needs inert gas shielding that cannot preserve for a long time.
Invention content
For the problem present on.The present invention proposes a kind of preparation method of the copper nanometer sheet of high stability, passes through
Copper ion salt and alkyl trimethyl quaternary ammonium salt type surfactant hybrid reaction in water, through reduction reaction, further detach
Purifying obtains state of aggregation fluorescence copper nanometer sheet.The preparation method is convenient, reaction condition temperature, without large-scale instrument, it can be achieved that batch
Production, the copper nanometer tablet stability of preparation is good, fluorescent emission intensity is controllable.
A kind of preparation method of the copper nanometer sheet of high stability of the present invention, this method are by copper ion salt and alkyl trimethyl
Copper nanometer sheet is prepared in quaternary ammonium salt cationic surfactant hybrid reaction in water, further reduction reaction, separating-purifying.
This method includes copper ion salt and the reaction of alkyl trimethyl quaternary ammonium salt type surfactant, reduction reaction, detaches and carries
Pure step；It is as follows：
(1) copper ion salt is reacted with alkyl trimethyl quaternary ammonium salt type surfactant：Weigh copper ion salt and alkyl front three
Based quaternary ammonium salt type surfactant adds in deionized water, stirring and dissolving, mixing time is 1-5 hours, stirring speed in reaction vessel
It spends for 500~2500rpm.A concentration of 0.005~the 5mol/ of alkyl trimethyl quaternary ammonium salt type surfactant in deionized water
The molar ratio example of L, copper ion salt and alkyl trimethyl quaternary ammonium salt type surfactant is 0.05~10:1；
(2) reduction reaction：It dissolves reduce agent in deionized water, is slowly dropped to (1) described solution, is stirred to react.Instead
It it is 0.5~24 hour between seasonable, mixing speed is 500~2000rpm.Reducing agent is 0.05~5 with copper ion salt molar ratio:
1。
(3) separating-purifying：(2) mixed liquor obtained is centrifuged, and must be precipitated.It repeats washing centrifugation three times, adds every time
5-10 milliliters of water are resuspended, and supernatant is abandoned in centrifugation.6000~15000g of centrifugal rotational speed, 0.1~1 hour time.Obtained product vacuum
Drying, as copper nanometer sheet.
The alkyl trimethyl quaternary ammonium salt type surfactant to can dissolve and containing there are three methyl, an alkyl in water
It is one or two or more kinds of in the halogen quaternary ammonium salt of long-chain, the copper ion salt be one kind in water-soluble bivalent cupric ion salt or
Two kinds or more, the reducing agent is the one or two or more kinds in water-soluble reducing agent.
The alkyl trimethyl quaternary ammonium salt type surfactant is specially：Cetyltrimethylammonium bromide, octadecyl
Trimethyl ammonium chloride, heptadecyl trimethylammonium bromide, heptadecyl trimethyl ammonium chloride, cetyl trimethylammonium bromide,
Hexadecyltrimethylammonium chloride, tetradecyltrimethylammonium bromide, tetradecyl trimethyl ammonium chloride, trimethyl
Ammonium chloride, dodecyl trimethyl ammonium bromide, ten alkyl trimethyl ammonium bromides, middle one kind of decyl trimethyl ammonium chloride or two
Kind or more.
The water-soluble copper ion salt, specially：Copper chloride, copper bromide, copper nitrate, one kind in copper acetate or two kinds
More than.
The water-soluble reducing agent includes：One or two or more kinds in ascorbic acid, hydrazine hydrate, sodium borohydride.
The present invention's has the following advantages that：
1. without large-scale instrument and equipment, manufacturing cost is low, and method is easy, and reaction condition is mild；
2. the copper nanometer tablet stability prepared is high, there is potential application in terms of the material preparations such as optics, electricity, catalysis
Value；
3. the fluorescence intensity of bronze medal nanometer sheet can by adjust copper ion salt, alkyl trimethyl quaternary ammonium salt type surfactant,
The ratio of reducing agent regulates and controls, and has potential using value in fields such as bio-imaging, sensing detections；
Description of the drawings
The transmission electron microscope picture of Fig. 1, copper nanometer sheet；
The transmission electron microscope picture of Fig. 2, copper nanometer sheet；
The scanning electron microscope (SEM) photograph of Fig. 3 copper nanometer sheets.
Specific implementation method
The above of the present invention is described in further details, but should not this be interpreted as this hair by the following examples
Bright to be limited only to following embodiment, every technology realized based on the content of present invention is regarded as the scope of the present invention.
A kind of preparation method of copper nanometer sheet is by copper ion salt and alkyl trimethyl quaternary ammonium salt type surfactant-dispersed
Hybrid reaction in deionized water adds in reducing agent reduction, isolated solid, further washing purifying, after vacuum drying
Obtain copper nanometer sheet.
Embodiment 1
36 milligrams of cetyl trimethylammonium bromides and 68 milligrams of Copper dichloride dihydrates are weighed in reaction vessel, add in 8 millis
Deionized water, stirring and dissolving are risen, mixing speed 1700rpm is stirred 30 minutes, and temperature is 25 DEG C.Weigh 3.8 milligrams of hydroborations
Sodium is dissolved in 2 ml deionized waters, is slowly dropped to above-mentioned mixed liquor, and solid is precipitated, continues to be stirred to react 1 hour.It obtains above-mentioned
Reaction solution is precipitated by centrifugation (12500g, 30 minutes).It adds in 10ml deionized waters and precipitation is resuspended, then centrifuge (12500g,
10 minutes) supernatant is abandoned, it must precipitate.Washing centrifugation three times is repeated, precipitates and copper nanometer sheet solid product is obtained after vacuum drying.Weight
Rehydration washes centrifugation three times, precipitates and copper nanometer sheet solid product is obtained after vacuum drying.Pass through scanning electron microscope (see Fig. 3) and transmission
Electronic Speculum (see Fig. 1, Fig. 2) is analysis shows obtained solid product is copper nanometer sheet.Obtained copper nanometer sheet is in 254nm ultraviolet lamps
Lower transmitting yellow fluorescence.
Embodiment 2
360 milligrams of cetyl trimethylammonium bromides and 112 milligrams of copper bromides are weighed in reaction vessel, 8 milliliters is added in and goes
Ionized water, stirring and dissolving, mixing speed 1700rpm are stirred 30 minutes, and temperature is 25 DEG C.It is molten to weigh 3.8 milligrams of sodium borohydrides
In 2 ml deionized waters, above-mentioned mixed liquor is slowly dropped to, solid is precipitated, continues to be stirred to react 1 hour.Obtain above-mentioned reaction
Liquid is precipitated by centrifugation (12500g, 30 minutes).It adds in 10ml deionized waters and precipitation is resuspended, then centrifuge (12500g, 10 points
Clock) supernatant is abandoned, it must precipitate.Washing centrifugation three times is repeated, precipitates and copper nanometer sheet solid product is obtained after vacuum drying.Further
The copper nanometer sheet obtained by scanning electron microscope and transmission electron microscope analysis.Obtained copper nanometer sheet emits orange under 254nm ultraviolet lamps
Color fluorescence.
Embodiment 3
32 milligrams of lauryl ammonium chlorides and 34 milligrams of Copper dichloride dihydrates are weighed in reaction vessel, add in 8 milliliters go from
Sub- water, stirring and dissolving, mixing speed 1000rpm are stirred 30 minutes, and temperature is 25 DEG C.7.6 milligrams of sodium borohydrides are weighed to be dissolved in
2 ml deionized waters are slowly dropped to above-mentioned mixed liquor, and solid is precipitated, continues to be stirred to react 1 hour.Obtain above-mentioned reaction solution
It is precipitated by centrifuging (12500g, 30 minutes).It adds in 10ml deionized waters and precipitation is resuspended, then centrifuge (12500g, 10 points
Clock) it must precipitate.Washing centrifugation three times is repeated, precipitates and copper nanometer sheet solid product is obtained after vacuum drying.Further by sweeping
Retouch the copper nanometer sheet that Electronic Speculum and transmission electron microscope analysis obtain.Obtained copper nanometer sheet emits fluorescent orange under 254nm ultraviolet lamps.
Embodiment 4
33 milligrams of tetradecyltrimethylammonium bromide are weighed with 68 milligrams of Copper dichloride dihydrates in reaction vessel, add in 8 millis
Deionized water, stirring and dissolving are risen, mixing speed 1700rpm is stirred 30 minutes, and temperature is 25 DEG C.Weigh 17 milligrams of Vitamin Cs
Acid is dissolved in 2 ml deionized waters, is slowly dropped to above-mentioned mixed liquor, and solid is precipitated, continues to be stirred to react 1 hour.It obtains above-mentioned
Reaction solution is precipitated by centrifugation (12500g, 30 minutes).It adds in 10ml deionized waters and precipitation is resuspended, then centrifuge (12500g,
10 minutes) it must precipitate.Washing centrifugation three times is repeated, precipitates and copper nanometer sheet solid product is obtained after vacuum drying.Further lead to
The copper nanometer sheet that overscanning Electronic Speculum and transmission electron microscope analysis obtain.
Embodiment 5
39 milligrams of Cetyltrimethylammonium bromides and 68 milligrams of Copper dichloride dihydrates are weighed in reaction vessel, add in 8 millis
Deionized water, stirring and dissolving are risen, mixing speed 1700rpm is stirred 30 minutes, and temperature is 40 DEG C.Weigh 3.8 milligrams of hydroborations
Sodium is dissolved in 2 ml deionized waters, is slowly dropped to above-mentioned mixed liquor, and solid is precipitated, continues to be stirred to react 1 hour.It obtains above-mentioned
Reaction solution is precipitated by centrifugation (12500g, 30 minutes).It adds in 10ml deionized waters and precipitation is resuspended, then centrifuge (12500g,
10 minutes) supernatant is abandoned, it must precipitate.Washing centrifugation three times is repeated, precipitates and copper nanometer sheet solid product is obtained after vacuum drying.Into
The copper nanometer sheet that one step is obtained by scanning electron microscope and transmission electron microscope analysis.Obtained copper nanometer sheet is issued in 254nm ultraviolet lamps
Penetrate yellow fluorescence.
Embodiment 6
34 milligrams of tetradecyltrimethylammonium bromide and 37 milligrams of copper nitrates are weighed in reaction vessel, add in 8 milliliters go from
Sub- water, stirring and dissolving, mixing speed 1700rpm are stirred 30 minutes, and temperature is 40 DEG C.3.8 milligrams of sodium borohydrides are weighed to be dissolved in
2 ml deionized waters are slowly dropped to above-mentioned mixed liquor, and solid is precipitated, continues to be stirred to react 1 hour.Obtain above-mentioned reaction solution
It is precipitated by centrifuging (12500g, 30 minutes).It adds in 10ml deionized waters and precipitation is resuspended, then centrifuge (12500g, 10 points
Clock) supernatant is abandoned, it must precipitate.Washing centrifugation three times is repeated, precipitates and copper nanometer sheet solid product is obtained after vacuum drying.Further
The copper nanometer sheet obtained by scanning electron microscope and transmission electron microscope analysis.
Embodiment 7
47 milligrams of decyl trimethyl ammonium chlorides and 36 milligrams of copper acetates are weighed in reaction vessel, add in 8 milliliters of deionizations
Water, stirring and dissolving, mixing speed 1700rpm are stirred 30 minutes, and temperature is 25 DEG C.It weighs 3.8 milligrams of sodium borohydrides and is dissolved in 2
Ml deionized water is slowly dropped to above-mentioned mixed liquor, and solid is precipitated, continues to be stirred to react 1 hour.Obtain above-mentioned reaction solution warp
Centrifugation (12500g, 30 minutes) is crossed to be precipitated.It adds in 10ml deionized waters and precipitation is resuspended, then centrifuge (12500g, 10 minutes)
Supernatant is abandoned, must be precipitated.Washing centrifugation three times is repeated, precipitates and copper nanometer sheet solid product is obtained after vacuum drying.Further lead to
The copper nanometer sheet that overscanning Electronic Speculum and transmission electron microscope analysis obtain.
Embodiment 8
67 milligrams of tetradecyltrimethylammonium bromide are weighed with 85 milligrams of Copper dichloride dihydrates in reaction vessel, add in 10 millis
Deionized water, stirring and dissolving are risen, mixing speed 1700rpm is stirred 30 minutes, and temperature is 25 DEG C.62.5 are pipetted with liquid-transfering gun
Microlitre 40% hydrazine hydrate is slowly dropped to above-mentioned mixed liquor, and solid is precipitated, continues to be stirred to react 1 hour.Obtain above-mentioned reaction solution
It is precipitated by centrifuging (12500g, 30 minutes).It adds in 10ml deionized waters and precipitation is resuspended, then centrifuge (12500g, 10 points
Clock) supernatant is abandoned, it must precipitate.Washing centrifugation three times is repeated, precipitates and copper nanometer sheet solid product is obtained after vacuum drying.Further
The copper nanometer sheet obtained by sweeping Electronic Speculum and transmission electron microscope analysis.
Claims (6)
1. the preparation method of the copper nanometer sheet of a kind of high stability, it is characterised in that this method is：Copper ion salt and alkyl front three
Copper nanometer sheet is prepared in based quaternary ammonium salt type surfactant hybrid reaction in water, further reduction reaction, separating-purifying.
2. the preparation method of the copper nanometer sheet of high stability according to claim 1, it is characterised in that this method include copper from
Alite is reacted with alkyl trimethyl quaternary ammonium salt type surfactant, reduction reaction, purification procedures；It is as follows：
(1) copper ion salt is reacted with alkyl trimethyl quaternary ammonium salt type surfactant：Weigh copper ion salt and alkyl trimethyl season
Ammonium salt type surfactant adds in deionized water, stirring and dissolving, mixing time is 1-5 hours, mixing speed 500 in container
~2500rpm；A concentration of 0.005~the 5mol/L of the alkyl trimethyl quaternary ammonium salt type surfactant in deionized water,
The molar ratio example of copper ion salt and alkyl trimethyl quaternary ammonium salt type surfactant is 0.05~10:1；
(2) reduction reaction：It dissolves reduce agent in deionized water, is slowly dropped to (1) described solution, is stirred to react；During reaction
Between for 0.5~24 hour, reaction temperature is 25 DEG C, and mixing speed is 500~2500rpm；Reducing agent and copper ion salt molar ratio
Example is 0.05~5:1；
(3) separating-purifying：The mixed liquor that (2) obtain is centrifuged, must be precipitated；It repeats washing centrifugation three times, adds 5- every time
10 milliliters of water are resuspended, and supernatant is abandoned in centrifugation；6000~15000g of centrifugal rotational speed, 0.1~1 hour time；Obtained product vacuum is done
It is dry, as copper nanometer sheet.
3. the preparation method of the copper nanometer sheet of high stability according to claim 1 or claim 2, it is characterised in that：The alkyl three
Methyl quaternary ammonium salt form surfactant to can dissolve and containing there are three in the halogen quaternary ammonium salt of methyl, long alkyl chain in water
One or two or more kinds, the copper ion salt are the one or two or more kinds in water-soluble bivalent cupric ion salt, and described goes back
Former agent is the one or two or more kinds in water-soluble reducing agent.
4. the preparation method of the copper nanometer sheet of high stability according to claim 3, it is characterised in that：The alkyl trimethyl
Quaternary ammonium salt cationic surfactant is specially：Cetyltrimethylammonium bromide, octadecyltrimethylammonium chloride, heptadecyl three
Methyl bromide ammonium, heptadecyl trimethyl ammonium chloride, cetyl trimethylammonium bromide, hexadecyltrimethylammonium chloride, ten
Tetraalkyl trimethylammonium bromide, tetradecyl trimethyl ammonium chloride, dodecyl trimethyl ammonium chloride, trimethyl bromine
Change the middle one or two or more kinds of ammonium, ten alkyl trimethyl ammonium bromides or decyl trimethyl ammonium chloride.
5. the preparation method of the copper nanometer sheet of high stability according to claim 3, it is characterised in that the water-soluble copper
Ion salt is specially：One or two or more kinds in copper chloride, copper bromide, copper nitrate or copper acetate.
6. the preparation method of the copper nanometer sheet of high stability according to claim 3, it is characterised in that the water-soluble reduction
Agent is ascorbic acid, the one or two or more kinds in hydrazine hydrate, sodium borohydride.
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| CN110153443A (en) * | 2019-07-11 | 2019-08-23 | 中国科学院深圳先进技术研究院 | A kind of copper nanometer sheet and its preparation method and application |
| CN110586953A (en) * | 2018-06-12 | 2019-12-20 | 本田技研工业株式会社 | High yield preparation of two-dimensional copper nanosheets |
| CN113059173A (en) * | 2021-03-23 | 2021-07-02 | 西北有色金属研究院 | Preparation method of foliated porous copper nanosheet |
| CN114346254A (en) * | 2022-01-21 | 2022-04-15 | 重庆科技学院 | Method for preparing nano copper powder in eutectic ionic liquid |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110586953A (en) * | 2018-06-12 | 2019-12-20 | 本田技研工业株式会社 | High yield preparation of two-dimensional copper nanosheets |
| JP2020023745A (en) * | 2018-06-12 | 2020-02-13 | 本田技研工業株式会社 | High-yield production of two-dimensional copper nano-sheet |
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| CN110586953B (en) * | 2018-06-12 | 2022-09-16 | 本田技研工业株式会社 | High yield preparation of two-dimensional copper nanosheets |
| CN110153443A (en) * | 2019-07-11 | 2019-08-23 | 中国科学院深圳先进技术研究院 | A kind of copper nanometer sheet and its preparation method and application |
| CN113059173A (en) * | 2021-03-23 | 2021-07-02 | 西北有色金属研究院 | Preparation method of foliated porous copper nanosheet |
| CN113059173B (en) * | 2021-03-23 | 2022-02-08 | 西北有色金属研究院 | Preparation method of foliated porous copper nanosheet |
| CN114346254A (en) * | 2022-01-21 | 2022-04-15 | 重庆科技学院 | Method for preparing nano copper powder in eutectic ionic liquid |
| CN114346254B (en) * | 2022-01-21 | 2023-08-18 | 重庆科技学院 | Method for preparing nanometer copper powder in eutectic ionic liquid |
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| CN108127125B (en) | 2020-01-14 |
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