CN107052358A - A kind of preparation method of copper nano-wire - Google Patents
A kind of preparation method of copper nano-wire Download PDFInfo
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- CN107052358A CN107052358A CN201611155853.8A CN201611155853A CN107052358A CN 107052358 A CN107052358 A CN 107052358A CN 201611155853 A CN201611155853 A CN 201611155853A CN 107052358 A CN107052358 A CN 107052358A
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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
- 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
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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 invention provides a kind of preparation method of copper nano-wire, comprise the following steps：A) Jiang Tongyuan, glucose, high fatty amine and water mixing, obtain mixed emulsion；B reacted after) mixed emulsion is heated, obtain first stage product；C it) will be reacted after the first stage product heats, obtain copper nano-wire；Step B) described in the temperature reacted be 50~90 DEG C, step C) described in the temperature reacted be 80~150 DEG C, and step B) reaction temperature be less than step C) reaction temperature.During copper nano-wire is prepared, the application is reacted by substep, and limits the temperature for often walking reaction, it is ensured that copper ion is fully reduced, and obtains the higher copper nano-wire of yield.
Description
Technical field
The present invention relates to the preparing technical field of nano material, more particularly to a kind of preparation method of copper nano-wire.
Background technology
One-dimensional metal material is because of its unique optics, electricity, thermodynamics, machinery and catalytic performance in modern nano science
With in occupation of important position, but high manufacturing cost and unstable characteristic turn into it in practical application in nanometer technology
In a main bottleneck.Copper as it is tellurian it is high enrich cheap element, be ideal in one-dimensional metal material
It is commercialized option.Therefore, development can apply to following inexpensive nano material and high monodispersity, the good stabilization of nano-device
The demand of the one-dimensional copper nano-wire of property and oxygen resistence is very urgent.
The preparation method of copper nano-wire is mainly solvent phase synthesi, vapour deposition process and template-mediated electrodeposition process.It is existing
Stage, vapour deposition process and template-mediated electrodeposition process are also not enough to realize industrialization, and copper prepared by solvent phase synthesi is received
Rice noodles then need to be chosen between yield and quality, nano wire often poor quality prepared by high yield synthetic method；And
The nano wire that high-quality preparation method is obtained but is frequently limited by the limited to low yield and yield.
The content of the invention
Present invention solves the technical problem that being to provide a kind of preparation method of copper nano-wire, the method that the application is provided can
Magnanimity prepares high-quality copper nano-wire.
In view of this, this application provides a kind of preparation method of copper nano-wire, comprise the following steps：
A), Jiang Tongyuan, glucose, high fatty amine and water mixing, obtain mixed emulsion；
B), reacted after the mixed emulsion is heated, obtain first stage product；
C), it will be reacted after the first stage product heats, obtain copper nano-wire；
Step B) described in the temperature reacted be 50~90 DEG C, step C) described in the temperature reacted be 80~150 DEG C, and
Step B) reaction temperature be less than step C) reaction temperature.
It is preferred that, step B) described in the temperature reacted be 65~80 DEG C, step C) described in the temperature reacted for 90~
120℃。
It is preferred that, step B) in, the time of the reaction is 12~48h；Step C) in, time of the reaction for 12~
48h。
It is preferred that, the mol ratio of copper source and the glucose is (1~3)：1, copper source and high fatty amine
Mol ratio is (1~5)：1, the mol ratio of copper source and water is (1~5)：1.
It is preferred that, the temperature of the mixing is 20~50 DEG C.
It is preferred that, step C) in, the heating is carried out under agitation, the speed of the stirring for 0~250 turn/
min。
It is preferred that, copper source is selected from Copper dichloride dihydrate, copper nitrate or anhydrous cupric chloride；The high fatty amine is ten
One kind in hexamine, octadecylamine and oleyl amine.
It is preferred that, step C) in, also include after the reaction：
Obtained reaction solution is centrifuged.
It is preferred that, the rotating speed of the centrifugation is 1000~5000 turns/min.
This application provides a kind of preparation method of copper nano-wire, this method is first by raw copper source, high fatty amine, Portugal
Grape sugar is mixed with water, obtains mixed emulsion, is reacted after mixed emulsion is heated, first stage product is obtained, by first rank
Reacted after section product heats, obtain copper nano-wire；The application utilizes the means of stepwise reaction, most copper ion is first converted into
Copper nano dot, then subsequent reactions are completed on the basis of copper nano dot, so that the yield of copper nano-wire is improved.Experiment
As a result show, the preparation method for the copper nano-wire that the application is provided can disposably prepare 50g copper nano-wires, and copper nano-wire line footpath
Uniformly, tens microns of length, draw ratio is up to 700~1000.
Brief description of the drawings
Fig. 1 is the electron scanning micrograph of copper nano-wire prepared by the embodiment of the present invention 1；
Fig. 2 is the transmission electron microscope photo of copper nano-wire prepared by the embodiment of the present invention 2；
Fig. 3 is the transmission electron microscope photo of copper nano-wire prepared by the embodiment of the present invention 3；
The copper nano-wire stoste in Large Copacity glass reaction kettle that Fig. 4 prepares for the present invention.
Embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, still
It should be appreciated that these descriptions are simply to further illustrate the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.
The embodiment of the invention discloses a kind of preparation method of copper nano-wire, comprise the following steps：
A), Jiang Tongyuan, glucose, high fatty amine and water mixing, obtain mixed emulsion；
B), reacted after the mixed emulsion is heated, obtain first stage product；
C), it will be reacted after the first stage product heats, obtain copper nano-wire；
Step B) described in the temperature reacted be 50~90 DEG C, step C) described in the temperature reacted be 80~150 DEG C, and
Step B) reaction temperature be less than step C) reaction temperature.
This application provides a kind of preparation method of copper nano-wire, this method is capable of the copper nano-wire of single sintering magnanimity,
And quality is higher.
Specifically, the application first mixes raw material, i.e., copper source, glucose, high fatty amine are mixed with water, mixed
Close emulsion；During this, copper source is preferably Copper dichloride dihydrate, copper nitrate or anhydrous cupric chloride, in some specific implementations
In example, copper source is preferably Copper dichloride dihydrate；The high fatty amine is preferably cetylamine, octadecylamine or oleyl amine, at certain
In a little embodiments, the high fatty amine is cetylamine.Copper source and the mol ratio of glucose are (1~3)：1, in some realities
Apply in example, the mol ratio of copper source and glucose is (1~2)：1.Copper source and the mol ratio of the high fatty amine are
(1~5)：1, in certain embodiments, copper source and the mol ratio (2~5) of the high fatty amine：1.Copper source and water
Mol ratio be (1~5)：1, in certain embodiments, the mol ratio of copper source and the water is (2~5)：1.In order that former
Material is well mixed, and the mode that the mixing is preferred to use dispersed with stirring is carried out, and the temperature of the mixing is preferably 20~50 DEG C.
After raw material mixing, mixed emulsion is heated to a lower temperature and reacted after a period of time by the application,
Obtain first stage product.During this, the temperature of the reaction is 50~90 DEG C, in certain embodiments, the reaction
Temperature is 65~80 DEG C, specifically, the temperature of the reaction can be 65 DEG C, 70 DEG C, 75 DEG C or 80 DEG C.The time of the reaction is excellent
Elect 12~48h as, in certain embodiments, the time of the reaction is 24~36h.
After first set reaction, the application will react after obtained first stage product heats, the temperature of the reaction
For 80~150 DEG C, in certain embodiments, the temperature of the reaction is 90~120 DEG C, specifically, the temperature of the reaction is
100 DEG C, 110 DEG C, 95 DEG C or 120 DEG C.The time of the reaction is 12~48h, in certain embodiments, the time of the reaction
For 24h~36h.The application is reacted the preparation of traditional copper nano-wire substep, during this, more than 85% copper ion
5nm copper nano dot is reduced to first, then subsequent reactions are completed on the basis of copper nano dot again, has obtained copper nanometer
Line, is improved its yield, at least improves 1.6 times.In above process, if obtaining the reaction temperature of first stage product
Too low, then the conversion of copper nano dot is insufficient, and reaction temperature is too high, then cannot get copper nano dot.If the overlong time of reaction,
Cause copper nano dot continued growth, the yield of final influence copper nano-wire.
Finally preferably obtained reaction solution is centrifuged by the application, to remove unnecessary high fatty amine and part
Accessory substance, obtains including the copper nano-wire stoste of copper nano-wire.The rotating speed of the centrifugation is 1000~5000 turns/min,
In some specific embodiments, the rotating speed of the centrifugation is 2000~4000 turns/min.
The preparation method for the copper nano-wire that the present invention is provided can disposably prepare 50g high-quality copper nano wires, and it prepares production
Amount is maximum in the prior art, and the multi-step mixing synthetic technology of the present invention stirs synthesis relative to one-step synthesis or not
Yield have greatly improved.Further, because the present invention uses the reactor of similar industrial reactor, thus very
It is readily applied to a large amount of productions of industrially scalable.Test result indicates that, copper nano-wire line footpath prepared by the present invention is uniform, length
Tens microns, draw ratio 700~1000, with extraordinary application potential.
For a further understanding of the present invention, the preparation method of the copper nano-wire provided with reference to embodiment the present invention is entered
Row is described in detail, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
50 DEG C circulate oil bath under, in 50L glass reaction kettles by 342g Copper dichloride dihydrates, 792g glucose with
2.7kg cetylamines dispersed with stirring is warming up to 75 DEG C of reaction 24h, then risen again in 40L deionized waters after obtained emulsion dispersion
Temperature to 120 DEG C of 150rpm stirring reactions 24h, last 2000rpm centrifugations, collection obtains 50g copper nano-wire products.
Embodiment 2
50 DEG C circulate oil bath under, in 50L glass reaction kettles by 342g Copper dichloride dihydrates, 396g glucose with
2.16kg cetylamines dispersed with stirring is warming up to 70 DEG C of reactions 24h, Ran Houzai in 40L deionized waters after obtained emulsion dispersion
100 DEG C of 150rpm stirring reactions 24h are warming up to, last 2000rpm centrifugations, collection obtains 50g copper nano-wire products.
Embodiment 3
50 DEG C circulate oil bath under, in 50L glass reaction kettles by 85.5g Copper dichloride dihydrates, 99g glucose with
0.54kg cetylamines dispersed with stirring is warming up to 65 DEG C of reactions 24h, Ran Houzai in 40L deionized waters after obtained emulsion dispersion
110 DEG C of 150rpm stirring reactions 36h are warming up to, last 2000rpm, which is collected by centrifugation, obtains 20g copper nano-wire products.
Fig. 1 is the electron scanning micrograph of copper nano-wire prepared by the embodiment of the present invention 1；Fig. 2 is implemented for the present invention
The transmission electron microscope photo of copper nano-wire prepared by example 2；Fig. 3 is the transmission of copper nano-wire prepared by the embodiment of the present invention 3
Electron micrograph；The copper nano-wire stoste in Large Copacity glass reaction kettle that Fig. 4 prepares for the present invention.By Fig. 1
~Fig. 3 understands that copper nano-wire line footpath prepared by the present invention is uniform, tens microns of length, and draw ratio is up to 700~1000；By Fig. 4
As can be seen that due to the reactor using similar industrial reactor, thus expansion scale is easy to, applied to industrially scalable
A large amount of productions.
The explanation of above example is only intended to the method and its core concept for helping to understand the present invention.It should be pointed out that pair
, under the premise without departing from the principles of the invention, can also be to present invention progress for those skilled in the art
Some improvement and modification, these are improved and modification is also fallen into the protection domain of the claims in the present invention.
The foregoing description of the disclosed embodiments, enables professional and technical personnel in the field to realize or using the present invention.
A variety of modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, it is of the invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The most wide scope caused.
Claims (9)
1. a kind of preparation method of copper nano-wire, comprises the following steps：
A), Jiang Tongyuan, glucose, high fatty amine and water mixing, obtain mixed emulsion；
B), reacted after the mixed emulsion is heated, obtain first stage product；
C), it will be reacted after the first stage product heats, obtain copper nano-wire；
Step B) described in the temperature reacted be 50~90 DEG C, step C) described in the temperature reacted be 80~150 DEG C, and step
B reaction temperature) be less than step C) reaction temperature.
2. preparation method according to claim 1, it is characterised in that step B) described in the temperature reacted be 65~80
DEG C, step C) described in the temperature reacted be 90~120 DEG C.
3. preparation method according to claim 1, it is characterised in that step B) in, time of the reaction for 12~
48h；Step C) in, the time of the reaction is 12~48h.
4. preparation method according to claim 1, it is characterised in that copper source and the mol ratio of the glucose are (1
~3)：1, the mol ratio of copper source and high fatty amine is (1~5)：1, the mol ratio of copper source and water is (1~5)：1.
5. preparation method according to claim 1, it is characterised in that the temperature of the mixing is 20~50 DEG C.
6. preparation method according to claim 1, it is characterised in that step C) in, the heating is entered under agitation
OK, the speed of the stirring is 0~250 turn/min.
7. preparation method according to claim 1, it is characterised in that copper source is selected from Copper dichloride dihydrate, copper nitrate
Or anhydrous cupric chloride；The high fatty amine is one kind in cetylamine, octadecylamine and oleyl amine.
8. preparation method according to claim 1, it is characterised in that step C) in, also include after the reaction：
Obtained reaction solution is centrifuged.
9. preparation method according to claim 8, it is characterised in that the rotating speed of the centrifugation is 1000~5000
Turn/min.
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| CN201611155853.8A CN107052358B (en) | 2016-12-14 | 2016-12-14 | Preparation method of copper nanowire |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107820337A (en) * | 2017-11-14 | 2018-03-20 | 杭州电子科技大学 | A kind of novel graphite alkene heating material |
| CN107828080A (en) * | 2017-11-09 | 2018-03-23 | 扬州大学 | A kind of preparation method of copper nano-wire compounded latex conductive sponge |
| CN108237232A (en) * | 2018-04-08 | 2018-07-03 | 电子科技大学中山学院 | It is a kind of using ferrous salt as the copper nano-wire preparation method of catalyst |
| CN108470603A (en) * | 2018-04-23 | 2018-08-31 | 天津大学 | A kind of preparation method of copper nano-wire transparent electrode |
| CN108526480A (en) * | 2018-03-16 | 2018-09-14 | 浙江大学 | A kind of method that low cost quickly prepares copper nano-wire |
| CN110090642A (en) * | 2019-03-07 | 2019-08-06 | 天津大学 | Copper-based bottom zinc oxide composite and its preparation method and application |
| CN110441360A (en) * | 2019-08-20 | 2019-11-12 | 浙江工业大学 | A kind of preparation method of one-dimensional copper nano-wire glucose sensor electrode material |
| CN111618315A (en) * | 2020-06-04 | 2020-09-04 | 厦门大学 | Preparation method of copper nanowire |
| CN112220130A (en) * | 2020-10-26 | 2021-01-15 | 西安工程大学 | PM 2.5-preventing copper nanowire mask and preparation method thereof |
| CN113083327A (en) * | 2021-04-06 | 2021-07-09 | 浙江加州国际纳米技术研究院台州分院 | Preparation method of copper-based heterogeneous hollow nanotube material |
| CN113707862A (en) * | 2021-08-26 | 2021-11-26 | 厦门大学 | Copper nanowire wound silicon-carbon composite material and preparation method and application thereof |
| CN113996799A (en) * | 2021-10-08 | 2022-02-01 | 郑州工程技术学院 | Preparation method of copper nano material |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107828080A (en) * | 2017-11-09 | 2018-03-23 | 扬州大学 | A kind of preparation method of copper nano-wire compounded latex conductive sponge |
| CN107820337A (en) * | 2017-11-14 | 2018-03-20 | 杭州电子科技大学 | A kind of novel graphite alkene heating material |
| CN108526480A (en) * | 2018-03-16 | 2018-09-14 | 浙江大学 | A kind of method that low cost quickly prepares copper nano-wire |
| CN108237232A (en) * | 2018-04-08 | 2018-07-03 | 电子科技大学中山学院 | It is a kind of using ferrous salt as the copper nano-wire preparation method of catalyst |
| CN108470603A (en) * | 2018-04-23 | 2018-08-31 | 天津大学 | A kind of preparation method of copper nano-wire transparent electrode |
| CN110090642A (en) * | 2019-03-07 | 2019-08-06 | 天津大学 | Copper-based bottom zinc oxide composite and its preparation method and application |
| CN110441360A (en) * | 2019-08-20 | 2019-11-12 | 浙江工业大学 | A kind of preparation method of one-dimensional copper nano-wire glucose sensor electrode material |
| CN111618315A (en) * | 2020-06-04 | 2020-09-04 | 厦门大学 | Preparation method of copper nanowire |
| CN112220130A (en) * | 2020-10-26 | 2021-01-15 | 西安工程大学 | PM 2.5-preventing copper nanowire mask and preparation method thereof |
| CN112220130B (en) * | 2020-10-26 | 2024-02-20 | 西安工程大学 | PM 2.5-preventing copper nanowire mask and preparation method thereof |
| CN113083327A (en) * | 2021-04-06 | 2021-07-09 | 浙江加州国际纳米技术研究院台州分院 | Preparation method of copper-based heterogeneous hollow nanotube material |
| CN113707862A (en) * | 2021-08-26 | 2021-11-26 | 厦门大学 | Copper nanowire wound silicon-carbon composite material and preparation method and application thereof |
| CN113996799A (en) * | 2021-10-08 | 2022-02-01 | 郑州工程技术学院 | Preparation method of copper nano material |
| CN113996799B (en) * | 2021-10-08 | 2024-02-02 | 郑州工程技术学院 | Preparation method of copper nanomaterial |
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