CN103658675A - Copper nanowire and preparation method thereof - Google Patents
Copper nanowire and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a copper nanowire and a preparation method of the copper nanowire. The method comprises the steps that (1) a copper salt solution is added into an alkali solution, the two solutions are mixed, and the concentration of copper ions in the mixed solution ranges from 1*10<-7>mol/L to 1*10<-5>mol/L; (2) a mixed solution of a reducing agent and a dispersing agent is prepared and added into the mixed solution obtained in the step (1); (3) the copper salt solution is dropwise added into the solution obtained in the step (2) under the conditions of magnetic stirring or ultrasonic dispersing, and reaction is conducted for 0.5-6 hours at the temperature of 40-90 DEG C; (4) products obtained in the step (3) are centrifugally separated and washed, and then the copper nanowire is obtained. The copper nanowire obtained based on the preparation method has the good dispersity and inoxidizability, the particle sizes of the obtained products are uniform, the length of the prepared copper nanowire ranges from 3 micrometers to 15 micrometers, the diameter of the prepared copper nanowire ranges from 20nm to 100nm, and the maximum square resistance value can reach 10.1 ohm per square.
Description
Technical field
The present invention relates to technical field of nano material, particularly relate to a kind of NANO CRYSTAL COPPER WIRE and preparation method thereof.
Background technology
The film of electronic product screen is made by indium tin oxide (ITO) at present, and its transparency is very high, for information, also has good conductibility.But ito thin film must pass through vapor deposition, and this process is very slow, and the equipment that contains ITO is easy to split, and in addition, indium is also a kind of rare earth element of costliness, and the price of every kilogram is up to 800 dollars of left and right.These problems all impel global scientist to find as possible more cost effective material, find and can be plated in more quickly or be printed on required material surface, form transparent conductive film cheaply.One of alternative of ito thin film is to use the ink of cheap metallic conduction nano wire, the transparent conductive film being particularly prepared into metal nanometer line ink.Have research group to find that conducting film prepared by nano metal line is back and forth after crooked 1000 times, it still can keep conductibility and shape.In contrast to this, the conductibility of ito thin film and structure will damaged after bending several times.Within 2013, first item screen will be appeared on the market by the thread mobile phone of silver nanoparticle, but silver is similar, still very expensive with indium, and every kilogram of price can reach 1400 dollars.And by contrast, the content of copper is very abundant, relatively cheap price in noble metal and extremely people's favor, at the comparable indium of nature content and silver sufficient more than 1,000 doubly, price is also cheaply many, and every kilogram is only 9 dollars.Research shows, NANO CRYSTAL COPPER WIRE is made thin-film material and for the film on electronic equipment and solar cell, had identical characteristic at present, and NANO CRYSTAL COPPER WIRE is made thin-film material cost and can significantly be reduced.NANO CRYSTAL COPPER WIRE is as a kind of novel nano structure---NANO CRYSTAL COPPER WIRE conductive film, and it can reduce the display manufacturing costs such as mobile phone, electronic reader and panel computer greatly, can help scientist to build folding electronic product simultaneously.
At present, for the synthetic Chinese scholars of nano metal line, for developing Nanometer Copper, launch numerous research work, continually developed new technology and new method.For example have bibliographical information approximately 60 ℃～100 ℃ prepared length 1～500 μ m with NANO CRYSTAL COPPER WIRE diameter 20～300nm; but the organic matter that need to add the ethylenediamine of high volatility; and need to add excessive alkali as (NaOH or KOH), need under argon gas or hydrogen shield, store.Also having bibliographical information to prepare NANO CRYSTAL COPPER WIRE pattern controlling agent used is diethylenetriamine, triethylene, tetramine or the TEPA etc. that irritant ammonia is smelly.The preparation method who reports in addition overlength NANO CRYSTAL COPPER WIRE need to use noble metal Au, Pd, Pt or Cu etc. and make catalyst.What in these methods, have need to add virose organic matter shape inducer (organic matter of ethylenediamine or diethylenetriamine etc.), and nano metal line uniformity is poor, and purity is lower, and synthetic method cost is higher, technique more complicated.The NANO CRYSTAL COPPER WIRE of preparing with derivant in prior art, its sheet resistance value is more than 1000 Ω/sq.
Summary of the invention
Based on this, the object of this invention is to provide a kind of NANO CRYSTAL COPPER WIRE and preparation method thereof.
Concrete technical scheme is as follows:
A preparation method for NANO CRYSTAL COPPER WIRE, comprises the steps:
(1) it is that in the 40-90 ℃ of concentration aqueous slkali that is 1-10mol/L, after mixing, in solution, the concentration of copper ion is 1 * 10 that the copper salt solution that is 0.0005-0.05mol/L by concentration joins temperature
-7～1 * 10
-5mol/L;
(2) mixed solution of preparation reducing agent and dispersant, then joins in the solution that step (1) obtains, and after mixing, in solution, the concentration of reducing agent is 1 * 10
-4～1 * 10
-1mol/L, the concentration of dispersant is 1 * 10
-9～1 * 10
-3mol/L;
(3) copper salt solution that compound concentration is 0.005-0.5mol/L is then added drop-wise to step (2) and obtains in solution under the condition of magnetic agitation or ultrasonic dispersion, and in mixed solution, the concentration of copper ion is 1 * 10
-4～1 * 10
-1mol/L, the concentration of alkali is 0.1-5.0mol/L, reaction 0.5-6h, reaction temperature is 40-90 ℃;
(4) product step (3) being obtained carries out centrifugation, washing, obtains described NANO CRYSTAL COPPER WIRE.
In an embodiment, the speed dripping in step (3) is 0.4-2.4mL/ minute therein.
In an embodiment, described mantoquita is copper chloride, stannous chloride, copper sulphate, copper nitrate, copper citrate or Schweinfurt green therein.
In an embodiment, described aqueous slkali is sodium hydroxide solution, potassium hydroxide solution or aqua calcis therein.
In an embodiment, described reducing agent is potassium borohydride, sodium borohydride, glucose or hydroxylamine hydrochloride or hydrazine hydrate therein.
In an embodiment, described dispersant is polyvinylpyrrolidone, C therein
13～C
16alkyl sulfonic acid, dodecyl sodium sulfate or lauryl sodium sulfate.
Another object of the present invention is to provide a kind of NANO CRYSTAL COPPER WIRE.
Concrete technical scheme is as follows:
The NANO CRYSTAL COPPER WIRE that above-mentioned preparation method prepares.
Therein in an embodiment, this Nanometer Copper line length 3～15 μ m, diameter is 20～100nm.
Principle of the present invention is as follows:
First utilize reducing agent to reduce rare mantoquita and prepare the nano copper particle crystal seed that particle diameter is little, use again seeded growth method, in reducing agent system, copper ion is reduced to Nanometer Copper and grows on a crystal face of copper, along with crystal face is constantly grown up and is become nano thread structure, the method is simple to operation, the demand of composite green environmental protection.Existing technology is to utilize organic matter derivant induction copper nano-particle to grow on a crystal face, and derivant used is low-boiling point material, volatile, and toxic.
Above-mentioned NANO CRYSTAL COPPER WIRE is expected to transparent conductive film being applied to electronic product etc., to substitute the ITO of present use.Compared with prior art, tool has the following advantages and beneficial effect in the present invention:
(1) the present invention is prepared in the aqueous solution, without organic solvent, meets saving, environmental protection demand;
(2) NANO CRYSTAL COPPER WIRE of the present invention has good dispersiveness and non-oxidizability, and the particle size were size obtaining is homogeneous comparatively, and prepared Nanometer Copper line length is 3～15 μ m, and diameter is between 20～100nm;
(3) can be by changing the concentration of crystal seed, the concentration of mantoquita and reaction temperature regulate and control length and the diameter of NANO CRYSTAL COPPER WIRE, prepared NANO CRYSTAL COPPER WIRE has lower resistance, and its sheet resistance minimum of a value can reach 10.1 Ω/;
(4) this method has that equipment is simple, raw material is cheap and easy to get, cost is low, and productive rate high is applicable to large-scale industrial production;
(5) by changing the size of NANO CRYSTAL COPPER WIRE, thereby prepare the NANO CRYSTAL COPPER WIRE that electric conductivity is different, then according to the different demands of electronic product, certain NANO CRYSTAL COPPER WIRE and mixed with resin are applied to the preparation of nesa coating, be expected to substitute the current electronic products such as conducting film with ITO or the preparation of silver slurry, at electronic applications, play an important role.
Accompanying drawing explanation
Fig. 1 is the XRD(X-x ray diffraction analysis x of NANO CRYSTAL COPPER WIRE) figure;
Fig. 2 is the SEM(SEM of embodiment 1 gained NANO CRYSTAL COPPER WIRE) shape appearance figure;
Fig. 3 is the SEM shape appearance figure of embodiment 2 gained NANO CRYSTAL COPPER WIRE;
Fig. 4 is the SEM shape appearance figure of embodiment 3 gained NANO CRYSTAL COPPER WIRE;
Fig. 5 is the SEM shape appearance figure of embodiment 4 gained NANO CRYSTAL COPPER WIRE;
Fig. 6 is the SEM shape appearance figure of embodiment 5 gained NANO CRYSTAL COPPER WIRE;
Fig. 7 is the SEM shape appearance figure of embodiment 6 gained NANO CRYSTAL COPPER WIRE;
Fig. 8 is the elementary analysis EDS(electron spectrum of NANO CRYSTAL COPPER WIRE) figure.
The specific embodiment
By the following examples the application is further elaborated.
Embodiment 1
The preparation method of the present embodiment NANO CRYSTAL COPPER WIRE, comprises the steps:
(1) aqua calcis of getting 0.5L1mol/L, in reactor, starts magnetic stirring apparatus and supersonic generator, is heated to 50 ℃, adds the Schweinfurt green solution of 20 μ L0.01mol/L and stirs;
(2) get 0.005mol/L solution of potassium borohydride 200mL and 1 * 10
-3after mol/L polyvinylpyrrolidonesolution solution 25mL mixes, join in the solution that step (1) obtains and stir;
(3) keep reaction 0.5 hour after adding the Schweinfurt green solution of 1L0.01mol/L with the speed of 2.0mL/ minute, reaction temperature is 50 ℃;
(4) product step (3) being obtained carries out centrifugation, uses absolute ethyl alcohol and distilled water washes clean, obtains described NANO CRYSTAL COPPER WIRE.
By above-mentioned product through X-ray diffraction analysis (XRD, as shown in Figure 1) and EDS(as shown in Figure 8) analyze as fine copper; The appearance structure of observing the present embodiment gained NANO CRYSTAL COPPER WIRE through SEM, as shown in Figure 2, visible, gained NANO CRYSTAL COPPER WIRE presents linear structure, and line length is 3～10 μ m, and linear diameter is 80～100nm; By four point probe resistance instrument test resistance, show that its NANO CRYSTAL COPPER WIRE square resistance is 100.8 Ω/.
Embodiment 2
The preparation method of the present embodiment NANO CRYSTAL COPPER WIRE, comprises the steps:
(1) sodium hydroxide solution of getting 0.2L5mol/L, in reactor, starts magnetic stirring apparatus and supersonic generator, is heated to 40 ℃, adds the copper-bath of 40 μ L0.0005mol/L and stirs;
(2) get 0.005mol/L sodium borohydride solution 10mL and 1 * 10
-3mol/LC
13～C
16after alkyl sulfonic acid sodium solution 20mL mixes, join in the solution that step (1) obtains, and stir;
(3) keep reaction 2 hours, 40 ℃ of reaction temperatures after adding the copper-bath of 1L0.05mol/L with the speed of 0.4mL/ minute;
(4) product step (3) being obtained is carried out centrifugation, and absolute ethyl alcohol and distilled water washes clean obtain the present embodiment NANO CRYSTAL COPPER WIRE.
It is similar to embodiment 1 that X-ray diffraction is analyzed (XRD) figure; The appearance structure of observing the present embodiment gained NANO CRYSTAL COPPER WIRE through SEM, as shown in Figure 3: visible, gained NANO CRYSTAL COPPER WIRE presents linear structure, line length is 6～15 μ m, linear diameter is 60～100nm, better dispersed; EDS figure is similar to embodiment 1; By four point probe resistance instrument test resistance, show that its NANO CRYSTAL COPPER WIRE square resistance is 79.1 Ω/.
Embodiment 3
The preparation method of the present embodiment NANO CRYSTAL COPPER WIRE, comprises the steps:
(1) potassium hydroxide solution of getting 0.1L8mol/L, in reactor, starts magnetic stirring apparatus and ultrasonic sound appratus, and is heated to 70 ℃, adds the copper nitrate solution of 60 μ L0.01mol/L and stirs;
(2) get 0.015mol/L glucose solution 300mL and 1 * 10
-4after mol/L lauryl sodium sulfate 15mL mixes, join in the solution that step (1) obtains, and stir;
(3) keep reaction 3 hours, 70 ℃ of reaction temperatures after adding the copper nitrate solution of 1L0.01mol/L with the speed of 1.2mL/ minute;
(4) product step (3) being obtained carries out centrifugation, by absolute ethyl alcohol and distilled water washes clean, obtains the present embodiment NANO CRYSTAL COPPER WIRE.
It is similar to embodiment 1 that X-ray diffraction is analyzed (XRD) figure; Through SEM, observe the appearance structure of the present embodiment gained NANO CRYSTAL COPPER WIRE, as shown in Figure 4: line length is 3～8 μ m, and linear diameter is 10～50nm, better dispersed; EDS figure is similar to embodiment; By four point probe resistance instrument test resistance, show that its NANO CRYSTAL COPPER WIRE square resistance is 20.3 Ω/.
Embodiment 4
The preparation method of the present embodiment NANO CRYSTAL COPPER WIRE, comprises the steps:
(1) sodium hydroxide solution of getting 0.5L1mol/L, in reactor, starts magnetic stirring apparatus and supersonic generator, is heated to 90 ℃, adds the copper citrate solution of 20 μ L0.01mol/L and stirs;
(2) get 0.5mol/L hydroxylamine hydrochloride solution 30mL and 1 * 10
-3after mol/L dodecyl sodium sulfate 30mL mixes, join in the solution that step (1) obtains, and stir;
(3) keep reaction 3 hours after adding the copper citrate solution of 1L0.01mol/L with the speed of 0.8mL/ minute, reaction temperature is 90 ℃;
(4) product step (3) being obtained carries out centrifugation, by absolute ethyl alcohol and distilled water washes clean, obtains the present embodiment NANO CRYSTAL COPPER WIRE.
It is similar to embodiment 1 that X-ray diffraction is analyzed (XRD) figure; Through SEM, observe the appearance structure of the present embodiment gained NANO CRYSTAL COPPER WIRE, as shown in Figure 5: line length is 10～15 μ m, and linear diameter is 30～80nm, better dispersed; EDS figure is similar to embodiment 1; By four point probe resistance instrument test resistance, show that its NANO CRYSTAL COPPER WIRE square resistance is 15.1 Ω/.
The preparation method of the present embodiment NANO CRYSTAL COPPER WIRE, comprises the steps:
(1) sodium hydroxide solution of getting 0.3L1mol/L, in reactor, starts magnetic stirring apparatus and supersonic generator, is heated to 80 ℃, adds the copper chloride solution of 40 μ L0.05mol/L and stirs;
(2) get 0.005mol/L hydrazine hydrate solution 25mL and 1 * 10
-3after mol/L polyvinylpyrrolidonesolution solution 25mL mixes, join in the solution that step (1) obtains, and stir;
(3) keep reaction 1 hour after adding the Schweinfurt green solution of 1L0.01mol/L with the speed of 0.7mL/ minute, reaction temperature is 80 ℃;
(4) three Hydrated copper chlorides are dissolved in distilled water and are mixed with 0.5mol/L solution, by 160mL, copper chloride solution dropwise joins in the solution that step (3) obtains, and drop rate is 30 droplets/minute; Reaction time is 3h;
(5) product step (4) being obtained carries out centrifugation, by absolute ethyl alcohol and distilled water washes clean, obtains this enforcement NANO CRYSTAL COPPER WIRE.
It is similar to embodiment 1 that X-ray diffraction is analyzed (XRD) figure; Through SEM, observe the morphosis of the present embodiment gained NANO CRYSTAL COPPER WIRE, as shown in Figure 6: visible, line length is 8～15 μ m, and linear diameter is 50～100nm, better dispersed; EDS figure is similar to embodiment 1; By four point probe resistance instrument test resistance, show that its NANO CRYSTAL COPPER WIRE square resistance is 10.1 Ω/.
Embodiment 6
The preparation method of the present embodiment NANO CRYSTAL COPPER WIRE, comprises the steps:
(1) sodium hydroxide solution of getting 0.5L1mol/L, in reactor, starts magnetic stirring apparatus and supersonic generator, is heated to 70 ℃, adds the copper-bath of 30 μ L0.01mol/L and stirs;
(2) get 0.001mol/L solution of potassium borohydride 200mL and 1 * 10
-4after mol/L polyvinylpyrrolidonesolution solution 25mL mixes, join in the solution that step (1) obtains, and stir;
(3) keep reaction 3 hours after adding the copper chloride solution of 1L0.01mol/L with the speed of 2.0mL/ minute, reaction temperature is 70 ℃;
(4) product step (4) being obtained carries out centrifugation, by absolute ethyl alcohol and distilled water washes clean, obtains the present embodiment NANO CRYSTAL COPPER WIRE.
It is similar to embodiment 1 that X-ray diffraction is analyzed (XRD) figure; Through SEM, observe the appearance structure of the present embodiment gained NANO CRYSTAL COPPER WIRE, as shown in Figure 7: visible, line length is 5～10 μ m, and linear diameter is 10～50nm, better dispersed; EDS figure is similar to embodiment 1; By four point probe resistance instrument test resistance, show that its NANO CRYSTAL COPPER WIRE square resistance is 12.4 Ω/.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (8)
1. a preparation method for NANO CRYSTAL COPPER WIRE, is characterized in that, comprises the steps:
(1) it is that in the 40-90 ℃ of concentration aqueous slkali that is 1-10mol/L, after mixing, in solution, the concentration of copper ion is 1 * 10 that the copper salt solution that is 0.0005-0.05mol/L by concentration joins temperature
-7～1 * 10
-5mol/L;
(2) mixed solution of preparation reducing agent and dispersant, then joins in the solution that step (1) obtains, and after mixing, in solution, the concentration of reducing agent is 1 * 10
-4～1 * 10
-1mol/L, the concentration of dispersant is 1 * 10
-9～1 * 10
-3mol/L;
(3) copper salt solution that compound concentration is 0.005-0.5mol/L is then added drop-wise to step (2) and obtains in solution under the condition of magnetic agitation or ultrasonic dispersion, and in mixed solution, the concentration of copper ion is 1 * 10
-4～1 * 10
-1mol/L, the concentration of alkali is 0.1-5.0mol/L, reaction 0.5-6h, reaction temperature is 40-90 ℃;
(4) product step (3) being obtained carries out centrifugation, washing, obtains described NANO CRYSTAL COPPER WIRE.
2. the preparation method of NANO CRYSTAL COPPER WIRE according to claim 1, is characterized in that, the speed dripping in step (3) is 0.4-2.4mL/ minute.
3. according to the preparation method of the NANO CRYSTAL COPPER WIRE described in claim 1-2 any one, it is characterized in that, described mantoquita is copper chloride, stannous chloride, copper sulphate, copper nitrate, copper citrate or Schweinfurt green.
4. according to the preparation method of the NANO CRYSTAL COPPER WIRE described in claim 1-2 any one, it is characterized in that, described aqueous slkali is sodium hydroxide solution, potassium hydroxide solution or aqua calcis.
5. according to the preparation method of the NANO CRYSTAL COPPER WIRE described in claim 1-2 any one, it is characterized in that, described reducing agent is potassium borohydride, sodium borohydride, glucose or hydroxylamine hydrochloride or hydrazine hydrate.
6. according to the preparation method of the NANO CRYSTAL COPPER WIRE described in claim 1-2 any one, it is characterized in that, described dispersant is polyvinylpyrrolidone, C
13～C
16alkyl sulfonic acid, dodecyl sodium sulfate or lauryl sodium sulfate.
7. the NANO CRYSTAL COPPER WIRE that described in claim 1-6 any one, preparation method prepares.
8. NANO CRYSTAL COPPER WIRE according to claim 7, is characterized in that, this Nanometer Copper line length 3～15 μ m, and diameter is 20～100nm.
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