CN104959622A - Synthesis method for copper nanowire with different length-diameter ratios - Google Patents
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Abstract
The invention relates to a synthesis method for a copper nanowire with different length-diameter ratios. The method includes the following steps that 1, a mixed water solution A of bivalent copper salt and glucose is prepared; 2, an absolute ethyl alcohol solution B of oleylamine and oleic acid is prepared; 3, an ethanol solution C of polyvinylpyrrolidone is prepared; 4, the solution A, the solution B and the solution C are mixed, diluted with water and then stirred for 2 h-12 h at the temperature of 30 DEG C-80 DEG C; and 5, a solution obtained in the step 4 is reacted for 4 h-24 h at the temperature of 100 DEG C-130 DEG C. The method overcomes the defects of high process complexity, high reaction temperature, low product yield, low product purity and the like of a present conventional synthesis method. The copper nanowire which is good in controllability and dispersity, large in length-diameter ratio and free of tail end particles can be obtained.
Description
Technical field
The present invention relates to one-dimensional metal nano material, particularly relate to a kind of synthetic method of copper nano-wire of different draw ratio.
Background technology
Copper nano-wire has in fields such as touch-screen, solar cell, wearable device, Organic Light Emitting Diodes prospect of more extensively using because of the flex capability of its high conductivity, high permeability and excellence, is considered to the transparent conductive material of new generation being expected to replace tin indium oxide (ITO).And synthesize the prerequisite that high-quality copper nano-wire is the transparent conductive material of processability excellence.
At present, the method for synthesizing copper nano-wire mainly contains:
1, comprise template, method of electrostatic spinning, vapour deposition process, solid phase reduction method etc. " hard ' method.Wherein, template take corresponding template as mould, after filling respective material, gone to control or guide nano material growth by material as main structure body by physics or chemical method, and carry out along with reaction, and template autophage falls, and then obtains specific morphology product.Its main feature is be no matter that the reaction controllability that occurs in gas phase or liquid phase is better, but is subject to previously prepared corresponding template limiting, and its Product yields is very limited, and its polycrystalline product weak point that to be also template main.Although method of electrostatic spinning energy continuous production nano wire, be easily subject to environmental factor if temperature, humidity, process control parameters are as voltage, flow velocity, and solution parameter is as the impact of the factor such as surface tension, viscosity.Vapour deposition process needs to complete in a vacuum, and condition is comparatively harsh.Solid phase reduction method needs to complete under the high temperature conditions, and energy consumption is large and efficiency is low.These " firmly " methods, or severe reaction conditions, complex steps, otherwise cost is higher, poor controllability, thus not easily realizes large-scale production.
2, current, " soft " method based on liquid solution is the main stream approach of synthesis copper nano-wire, mainly comprises hydrothermal reduction method and solvent-thermal method etc.Although these methods have, cost is lower, controllability good, easily realize the advantages such as large-scale production, but also there is many technical problems respectively: adopt hydrothermal reduction method synthesis copper nano-wire, its synthesis step is comparatively loaded down with trivial details, the copper nano-wire terminal be synthesized has particle, have impact on the photoelectric properties of film.And although solvent-thermal method is simple to operate, usually under higher temperature (>150 DEG C), and need just can complete under inert gas shielding.
Chinese patent 201080062895.1 reports liquid phase reduction and prepares copper nano-wire, its copper nano-wire diameter 100 ± 10nm, and terminal is with particle, can affect film conductivity and transmitance.
Chinese patent 201110144380.2 has prepared monocrystal copper nanowires by liquid phase reduction, and because reactant concentration is low, it yields poorly.
Chinese patent 201210323822.4 reports the synthetic method of overlong nanowire (1500 μm), which uses noble metal as catalyst, and reaction temperature higher (190 DEG C).
Chinese patent 201410346038.4 reports the synthetic method of the copper nano-wire that draw ratio is large, purity is high, and it also completes synthesis under higher temperature (150 DEG C).
Chinese patent 201410362522.6 reports continuous seepage and is combined to copper nano-wire, although its productive rate is higher, synthesis step is loaded down with trivial details, and the copper nano-wire terminal of preparation is with particle.
Summary of the invention
The object of the present invention is to provide a kind of synthetic method of copper nano-wire of different draw ratio, this synthetic method overcomes the complex process existed in current conventional synthesis process, the shortcoming such as reaction temperature is high, Product yields low-purity is low, can obtain that controllability is good, draw ratio is large, good dispersion, and the agranular copper nano-wire of terminal.
The present invention is achieved through the following technical solutions above-mentioned technical purpose:
A synthetic method for the copper nano-wire of different draw ratio, is characterized in that, it carries out according to following steps:
(1) the mixed aqueous solution A of cupric salt and glucose is prepared;
(2) the ethanol solution B of oleyl amine and oleic acid is prepared;
(3) the ethanolic solution C of polyvinylpyrrolidone (PVP) is prepared;
(4) A, B and C are mixed, after dilute with water, at 30 ~ 80 DEG C, stir 2 ~ 12h;
(5) gained solution in step (4) is reacted 4 ~ 24h at 100 ~ 130 DEG C.
In order to be further purified obtained copper nano-wire, the synthetic method of the copper nano-wire of above-mentioned different draw ratio, also include step (6): reacted the solution n-hexane of rear gained and the mixed liquor of isopropyl alcohol by step (5), at 8000 ~ 12000rpm/min centrifuge washing for several times, be dispersed in isopropyl alcohol.
Above-mentioned cupric salt, specifically may be selected to be copper chloride, copper sulphate, Schweinfurt green or copper nitrate.
The consumption of the cupric salt in above-mentioned synthetic method, glucose, oleyl amine, oleic acid and PVP, configures according to following mol ratio: cupric salt: glucose: oleyl amine: oleic acid: PVP=1:0.5 ~ 2:4 ~ 8:0.05 ~ 0.12:0.5 ~ 2.2.As further preferred, it specifically configures according to following mol ratio: cupric salt: glucose: oleyl amine: oleic acid: PVP=1:1:6:0.06:1.1.
Above-mentioned polyvinylpyrrolidone, preferable weight-average molecular weight is the one in 55000,360000 or 1300000.
In the ethanolic solution C of the PVP prepared in above-mentioned steps (3), the mass fraction of PVP is 2% ~ 7%.
As further optimizing, the synthetic method of the copper nano-wire of above-mentioned different draw ratio, specifically carry out according to following steps:
(1) take 1.7 ~ 6.8g copper chloride and 1.98 ~ 7.92g glucose, add 500ml deionized water, stirred at ambient temperature evenly obtains blue solution A;
(2) measure 20 ~ 80ml oleyl amine, 20 ~ 80 μ l oleic acid and 140ml absolute ethyl alcohol, stirred at ambient temperature evenly obtains mixed liquid B;
(3) take PVP 5 ~ 20g that relative molecular mass is 55000, add 50ml absolute ethyl alcohol and stirring evenly, obtain mixed liquor C;
(4) by above-mentioned A, B and C mixing, be diluted to 1000 ~ 4000ml by deionized water, at 30 ~ 80 DEG C, add thermal agitation 2 ~ 12h, obtain cinerous solution;
(5) gained solution in step (4) is transferred in reactor, at 110 ~ 130 DEG C, react 4 ~ 24h; Wherein, control the time that reaction is different, can obtain the copper nano-wire of different draw ratio, the reaction time is longer, and the copper nano-wire draw ratio obtained is larger;
(6) naturally cooled by the solution of gained after reacting completely in step (5), be the n-hexane of 0.5 ~ 2:1 and the mixed liquor of isopropyl alcohol by volume ratio, under 8000 ~ 12000rpm/min condition, centrifuge washing 4 times, is dispersed in isopropyl alcohol.
The inventive method has the following advantages:
(1) the method is simple, controllability good, easy and simple to handle, with low cost, output is high, be easy to batch production;
(2) the method is by only changing the reaction time, and can obtain the copper nano-wire of different draw ratio, and the diameter of its product is at 30 ~ 100nm, controlled in length 20 ~ 120 μm;
(3) the product copper nano-wire adopting the method obtained, its pattern evenly, terminal without particle, good dispersion, after centrifuge washing, has extensive utilization prospect in transparent conductive material field.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the copper nano-wire of synthesis in the embodiment of the present invention 1.
Fig. 2 is SEM (SEM) figure of the copper nano-wire of synthesis in the embodiment of the present invention 1.
Fig. 3 is the absorption spectrogram of the copper nano-wire dispersion liquid of synthesis in the embodiment of the present invention 1.
Fig. 4 is the transmission electron microscope of copper nano-wire under different amplification (TEM) figure of synthesis in the embodiment of the present invention 1.
Fig. 5-7 is the SEM figure of copper nano-wire under different amplification of synthesis in the embodiment of the present invention 1.
Fig. 8 is the SEM figure of the copper nano-wire of synthesis in the embodiment of the present invention 2.
Fig. 9 is the TEM figure of the copper nano-wire of synthesis in the embodiment of the present invention 2.
Figure 10-12 is the SEM figure of copper nano-wire under different amplification of synthesis in the embodiment of the present invention 2.
Figure 13 is the SEM figure of the copper nano-wire of synthesis in the embodiment of the present invention 3.
Figure 14 is the TEM figure of the copper nano-wire of synthesis in the embodiment of the present invention 3.
Detailed description of the invention
Below by embodiment, the present invention is specifically described; but following examples are only for being further detailed the present invention; can not be interpreted as the restriction to its protection domain, the person skilled in the art in this field can make some nonessential improvement and adjustment according to foregoing to the present invention.
Embodiment 1
A synthetic method for the copper nano-wire of different draw ratio, it carries out according to following steps:
(1) take the copper chloride of 0.02mol and the glucose of 0.02mol, dissolve under adding 1000ml deionized water room temperature and stir, obtain blue solution A;
(2) 40ml oleyl amine, 40 μ l oleic acid are measured, and 70ml absolute ethyl alcohol, stirred under room temperature and be mixed with mixed liquid B;
(3) configuring 20ml mass fraction is the PVP(Mw=360000 of 3%)-ethanolic solution C;
(4) A, B and C are mixed, after deionized water dilution, under 80 DEG C of conditions, heat magnetic agitation 5h;
(5) gained solution in step (4) is proceeded in reactor, at 120 DEG C, react 6h;
(6) solution having reacted rear gained in step (5) is cooled naturally, be the hexane of 2:1 and the mixed liquor of isopropyl alcohol by volume ratio more afterwards, 8000rpm/min centrifuge washing 4 times, by isopropanol, namely obtains disperseing good copper nano-wire dispersion liquid.
1 ~ 7 is known with reference to the accompanying drawings, and what this method obtained is pure face-centred cubic copper nano-wire; The length of this copper nano-wire is at 40 ~ 60 μm, and diameter is at 60 ~ 80nm, and this copper nano-wire does not have terminal particle.
Embodiment 2
A synthetic method for the copper nano-wire of different draw ratio, it carries out according to following steps:
(1) take the copper chloride of 0.04mol and the glucose of 0.04mol, dissolve under adding 2000ml deionized water room temperature and stir, obtain blue solution A;
(2) 80ml oleyl amine, 80 μ l oleic acid are measured, and 140ml absolute ethyl alcohol, stirred under room temperature and be mixed with mixed liquid B;
(3) configuring 40ml mass fraction is the PVP(Mw=55000 of 3%)-ethanolic solution C;
(4) A, B and C are mixed, after deionized water dilution, under 50 DEG C of conditions, heat magnetic agitation 8h;
(5) gained solution in step (4) is proceeded in reactor, at 120 DEG C, react 12h;
(6) solution having reacted rear gained in step (5) is cooled naturally, be the hexane of 1:1 and the mixed liquor of isopropyl alcohol by volume ratio more afterwards, 12000rpm/min centrifuge washing 4 times, by isopropanol, namely obtains disperseing good copper nano-wire dispersion liquid.
8 ~ 12 is known with reference to the accompanying drawings, and the copper nano-wire internal structure that this method obtains is continuous, size is comparatively even; The length of this copper nano-wire is at 80 ~ 100 μm, and diameter is at 30 ~ 45nm, and this copper nano-wire does not have terminal particle.
Embodiment 3
A synthetic method for the copper nano-wire of different draw ratio, it carries out according to following steps:
(1) take the copper chloride of 0.02mol and the glucose of 0.02mol, dissolve under adding 1000ml deionized water room temperature and stir, obtain blue solution A;
(2) 40ml oleyl amine, 40 μ l oleic acid are measured, and 70ml absolute ethyl alcohol, stirred under room temperature and be mixed with mixed liquid B;
(3) configuring 20ml mass fraction is the PVP(Mw=1300000 of 3%)-ethanolic solution C;
(4) A, B and C are mixed, after deionized water dilution, under 60 DEG C of conditions, heat magnetic agitation 7h;
(5) gained solution in step (4) is proceeded in reactor, at 110 DEG C, react 4h;
(6) solution having reacted rear gained in step (5) is cooled naturally, be the hexane of 0.5:1 and the mixed liquor of isopropyl alcohol by volume ratio more afterwards, 12000rpm/min centrifuge washing 4 times, by isopropanol, namely obtains disperseing good copper nano-wire dispersion liquid.
13 and 14 is known with reference to the accompanying drawings, and the length of this copper nano-wire is at 10 ~ 25 μm, and diameter is at 90 ~ 110nm, and this copper nano-wire does not have terminal particle.
Embodiment 4
A synthetic method for the copper nano-wire of different draw ratio, it carries out according to following steps:
(1) take the copper nitrate of 0.02mol and the glucose of 0.02mol, dissolve under adding 1200ml deionized water room temperature and stir, obtain blue solution A;
(2) 40ml oleyl amine, 40 μ l oleic acid are measured, and 80ml absolute ethyl alcohol, stirred under room temperature and be mixed with mixed liquid B;
(3) configuring 20ml mass fraction is the PVP(Mw=1300000 of 7%)-ethanolic solution C;
(4) A, B and C are mixed, after deionized water dilution, under 40 DEG C of conditions, heat magnetic agitation 10h;
(5) gained solution in step (4) is proceeded in reactor, at 130 DEG C, react 5h;
(6) solution having reacted rear gained in step (5) is cooled naturally, be the n-hexane of 1.5:1 and the mixed liquor of isopropyl alcohol by volume ratio more afterwards, 10000rpm/min centrifuge washing 3 times, by isopropanol, namely obtains disperseing good copper nano-wire dispersion liquid.
Claims (7)
1. a synthetic method for the copper nano-wire of different draw ratio, is characterized in that, it carries out according to following steps:
(1) the mixed aqueous solution A of cupric salt and glucose is prepared;
(2) the ethanol solution B of oleyl amine and oleic acid is prepared;
(3) the ethanolic solution C of polyvinylpyrrolidone is prepared;
(4) A, B and C are mixed, after dilute with water, at 30 ~ 80 DEG C, stir 2 ~ 12h;
(5) gained solution in step (4) is reacted 4 ~ 24h at 100 ~ 130 DEG C.
2. the synthetic method of the copper nano-wire of different draw ratio as claimed in claim 1, it is characterized in that, it also includes step (6): reacted the solution n-hexane of rear gained and the mixed liquor of isopropyl alcohol by step (5), at 8000 ~ 12000rpm/min centrifuge washing for several times, be dispersed in isopropyl alcohol.
3. the synthetic method of the copper nano-wire of different draw ratio as claimed in claim 1 or 2, is characterized in that: described cupric salt is chosen as copper chloride, copper sulphate, Schweinfurt green or copper nitrate.
4. the synthetic method of the copper nano-wire of different draw ratio as described in as arbitrary in claim 1-3, it is characterized in that, the consumption of cupric salt wherein, glucose, oleyl amine, oleic acid and polyvinylpyrrolidone, configures according to following mol ratio: cupric salt: glucose: oleyl amine: oleic acid: polyvinylpyrrolidone=1:0.5 ~ 2:4 ~ 8:0.05 ~ 0.12:0.5 ~ 2.2.
5. the synthetic method of the copper nano-wire of different draw ratio as described in as arbitrary in claim 1-3, it is characterized in that, the consumption of cupric salt wherein, glucose, oleyl amine, oleic acid and polyvinylpyrrolidone, configures according to following mol ratio: cupric salt: glucose: oleyl amine: oleic acid: polyvinylpyrrolidone=1:1:6:0.06:1.1.
6. the synthetic method of the copper nano-wire of different draw ratio as described in as arbitrary in claim 1-5, is characterized in that: it is one in 55000,360000 or 1300000 that described polyvinylpyrrolidone is chosen as weight average molecular weight; In the ethanolic solution C of the polyvinylpyrrolidone prepared in described step (3), the mass fraction of polyvinylpyrrolidone is 2% ~ 7%.
7. the synthetic method of the copper nano-wire of different draw ratio as claimed in claim 1, it is characterized in that, it specifically carries out according to following steps:
(1) take 1.7 ~ 6.8g copper chloride and 1.98 ~ 7.92g glucose, add 500ml deionized water, stirred at ambient temperature evenly obtains blue solution A;
(2) measure 20 ~ 80ml oleyl amine, 20 ~ 80 μ l oleic acid and 140ml absolute ethyl alcohol, stirred at ambient temperature evenly obtains mixed liquid B;
(3) take polyvinylpyrrolidone 5 ~ 20g that relative molecular mass is 55000, add 50ml absolute ethyl alcohol and stirring evenly, obtain mixed liquor C;
(4) by above-mentioned A, B and C mixing, be diluted to 1000 ~ 4000ml by deionized water, at 30 ~ 80 DEG C, add thermal agitation 2 ~ 12h, obtain cinerous solution;
(5) gained solution in step (4) is transferred in reactor, at 110 ~ 130 DEG C, react 4 ~ 24h;
(6) naturally cooled by the solution of gained after reacting completely in step (5), be the n-hexane of 0.5 ~ 2:1 and the mixed liquor of isopropyl alcohol by volume ratio, under 8000 ~ 12000rpm/min condition, centrifuge washing 4 times, is dispersed in isopropyl alcohol.
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| CN108376587A (en) * | 2018-03-07 | 2018-08-07 | 重庆文理学院 | A kind of high-performance stablizes the preparation method of copper nano-wire flexible transparent conductive film |
| CN108436104A (en) * | 2018-06-05 | 2018-08-24 | 黔南民族师范学院 | - kind of the technique for preparing copper nano-wire with acidic etching waste liquid |
| CN110355379A (en) * | 2019-07-31 | 2019-10-22 | 江苏大学 | A kind of difference draw ratio NANO CRYSTAL COPPER WIRE and its synthetic method |
| CN114603154A (en) * | 2022-03-22 | 2022-06-10 | 武汉纺织大学 | Preparation method of copper nanowire and copper nanowire prepared by same |
| CN115464133A (en) * | 2022-08-26 | 2022-12-13 | 深圳先进电子材料国际创新研究院 | Copper nanowire and preparation method thereof |
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| CN107052358A (en) * | 2016-12-14 | 2017-08-18 | 中国科学技术大学 | A kind of preparation method of copper nano-wire |
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| CN107103945A (en) * | 2017-06-23 | 2017-08-29 | 合肥工业大学 | A kind of copper nano-wire transparent conductive film and preparation method |
| CN108376587A (en) * | 2018-03-07 | 2018-08-07 | 重庆文理学院 | A kind of high-performance stablizes the preparation method of copper nano-wire flexible transparent conductive film |
| CN108436104A (en) * | 2018-06-05 | 2018-08-24 | 黔南民族师范学院 | - kind of the technique for preparing copper nano-wire with acidic etching waste liquid |
| CN110355379A (en) * | 2019-07-31 | 2019-10-22 | 江苏大学 | A kind of difference draw ratio NANO CRYSTAL COPPER WIRE and its synthetic method |
| CN114603154A (en) * | 2022-03-22 | 2022-06-10 | 武汉纺织大学 | Preparation method of copper nanowire and copper nanowire prepared by same |
| CN115464133A (en) * | 2022-08-26 | 2022-12-13 | 深圳先进电子材料国际创新研究院 | Copper nanowire and preparation method thereof |
| CN115464133B (en) * | 2022-08-26 | 2024-03-19 | 深圳先进电子材料国际创新研究院 | Copper nanowire and preparation method thereof |
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