CN110434353A - A kind of preparation method and applications of ball chain shape copper nano-wire - Google Patents
A kind of preparation method and applications of ball chain shape copper nano-wire Download PDFInfo
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- CN110434353A CN110434353A CN201910721230.XA CN201910721230A CN110434353A CN 110434353 A CN110434353 A CN 110434353A CN 201910721230 A CN201910721230 A CN 201910721230A CN 110434353 A CN110434353 A CN 110434353A
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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
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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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
- 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
- B22F1/0553—Complex form nanoparticles, e.g. prism, pyramid, octahedron
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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
- 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
- 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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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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Abstract
A kind of preparation method of the copper nano-wire of ball chain shape, which comprises the following steps: step 1: in deionized water by mantoquita dissolution, the trisodium citrate of equimolar amounts is then added thereto again, stirs evenly；Step 2: the pH value of solution in step 1 being adjusted to 9-11, suitable growth regulator is then added and is mixed；Step 3: the solution in step 2 being placed in oil bath pan, and reacts oil bath pan heating reaction system to certain temperature；Step 4: after the temperature of water-bath reaches set temperature, then suitable reducing agent being added into reaction system, and maintain to react 5-8h at such a temperature；After reaction, carrying out centrifuge washing to it can be obtained the copper nano-wire of product ball chain shape.
Description
Technical field
The present invention relates to a kind of preparation fields of flexible electronics, and in particular to a kind of preparation neck of flexible transparent electrode
Domain, especially a kind of preparation method and applications field of ball chain shape copper nano-wire.
Background technique
In recent years, with the fast development of electronic industry, with flexible electronic, wearable device, transparent heater part, intelligence
Household is the rapid appearance of the emerging product of representative, so that market produces huge demand sky for flexible and transparent conductive electrode
Between.This is but also produce the flexible and transparent conductive electrode of high quality, high stability and low cost either in market still in section
Boundary's tool is ground to have very important significance.
Currently, the preparation about flexible and transparent conductive electrode is mainly with tin indium oxide (ITO) for main functional component,
In addition, further including AZO, FTO etc..This kind of material has similar property, and the mainstream conductive material on existing market in this way has
The features such as mature preparation process is stable, surface resistance is smaller, visible-light absorptivity is low, still, also have the shortcomings that it is very important,
If its brittleness is larger, the flexible of flexible device is limited, the reserves of raw ore are sharply reduced, so that the price of above-mentioned material
It is to get promotion continuously, further, since indium is a kind of toxic metals, this makes in the extractive process of raw ore, also will cause very big
Environmental pollution.Therefore, with the continuous development of nano material, sight has also been turned to searching by scientific research personnel can substitute above-mentioned material
The new function material of material.
In numerous candidate materials, study relatively broad has carbon material and metal nanometer line two major classes at present, wherein
Carbon material specifically includes that based on graphene, carbon nanotube and carbon nano-fiber, especially the most extensive with the research of graphene；
Such as 2010, South Korea's Samsung and the researcher at Jun Guan university realized large-sized Flexible graphene transparent conductive film
Preparation, and be used for flexible touch screen manufacture (referring to: SuKang Bae et al. is published in " Nature
Nanotechnology " on article " Roll-to-Roll production of 30-inch graphene films for
Transparent electrodes ").Later, in 2013, it is transparent that Sony Corporation of Japan also achieves large-sized graphene
The preparation of conductive film, has prepared the graphene film of maximum length about 120m wide about 230mm, and this graphene can answer
The fields such as flexible transparent electrode, Flexible Displays are used, show preferable performance (referring to Toshiyuki Kabayashi
Et al. be published in article " Production of a 100-m-long high-quality on " Appl.Phys.Lett. "
grapheme transparent conductive film by roll-to-roll chemical vapor
Deposition and transfer process ").And domestic Changzhou two dimension carbon Science and Technology Co., Ltd. and middle section
The research institutions such as Chongqing research institute, institute and Peking University also realize the life of large-area graphene film in the almost same time
It produces, but carbon material there are itself extinctions strong, the big drawback of contact resistance, this is that can not connect for high performance transparent conductive material
It receives.And metal nanometer line can avoid the above problem well, the metal nanometer line of present most study mainly includes silver
Nano wire and copper nano-wire, silver nanowires have good conductive, thermally conductive and stability, it is considered to be are hopeful very much to substitute
One of conductive material of ITO, but its higher cost, this makes the price of end product higher；And copper nano-wire has due to it
The electric conductivity similar with silver nanowires, but its cost is lower than silver nanowires from far away, therefore, using copper nano-wire as a kind of efficient
Transparent conductive material to study be a kind of reasonable selection, such as (be published in referring to Aaron R.Rathmell et al.
Article " The Growth Mechanism of Copper Nanowires and Their on " Adv.Mater. "
Properties in Flexible, Transparent Conducting Films ".
The quality of final products performance is largely dependent on the selection of raw material.Likewise, copper nano-wire is high-quality
The bad performance for also directly affecting transparent conductive electrode.And the main method for preparing copper nano-wire at present includes: physical method and change
Method, wherein chemical method mainly includes liquid phase synthesizing method, complementary field auxiliary law etc., as Fei Meng et al. is published in " Nano
Letters " on article " The Solution Growth of Copper Nanowires and Nanotubes is
Driven by Screw Dislocations " is coverture using EDA, and hydrazine hydrate is reducing agent, the use of copper nitrate is copper
Source adjusts the pH of reaction system by NaOH, and then the copper nano-wire of high quality can be obtained in hydro-thermal reaction.
Summary of the invention
It is an object of the invention to provide a kind of preparation method of the copper nano-wire of ball chain shape by adjusting reaction process,
And it is applied to the preparation of transparent conductive electrode, overcome the problems, such as that existing linear type copper nano-wire contact resistance is larger.
In order to make technical solution of the present invention familiar to those skilled in the art, now technical solution of the present invention is carried out as follows
Detailed description.
A kind of preparation method of the copper nano-wire of ball chain shape comprising following steps:
Step 1: in deionized water by mantoquita dissolution, the trisodium citrate of equimolar amounts is then added thereto again, stirring is equal
It is even；
Step 2: the pH value of solution in step 1 being adjusted to 9-11, suitable growth regulator is then added and is mixed；
Step 3: the solution in step 2 being placed in oil bath pan, and so that oil bath pan is heated reaction system to certain temperature and carries out instead
It answers；
Step 4: after the temperature of water-bath reaches set temperature, then suitable reducing agent being added into reaction system, and maintain
5-8h is reacted at such a temperature；After reaction, carrying out centrifuge washing to it can be obtained the copper nano-wire of product ball chain shape.
Preferably, the mantoquita in step 1 of the present invention refers to one of copper sulphate, copper nitrate, copper acetate or copper chloride.
Preferably, pH adjusting agent is one of sodium hydroxide, potassium hydroxide or calcium hydroxide or several in step 2 of the present invention
Kind.
Preferably, growth regulator refers to PVPK30 and CTAB in step 2 of the present invention.
Preferably, certain temperature refers to 110-120 DEG C in step 3 of the present invention.
Preferably, reducing agent used in step 4 of the present invention refers to or mixtures thereof sodium borohydride, hydrazine hydrate.
Preferably, if the reducing agent used in step 4 of the present invention is the mixture of the good hydrazine hydrate of sodium borohydride, it is also necessary to add
Add suitable alkaline matter.
Preferably, ball chain shape copper nano-wire prepared by the present invention is used for the preparation of transparent conductive electrode.And it is visited using four
Needle resistance instrument and UV-Visible spectrophotometer test the property of its surface resistance and light transmittance.
Compared with prior art, the present invention achieves following beneficial technical effect:
1) the uniform ball chain shape copper nano-wire of structure has been prepared by simple liquid phase synthesizing method；Its diameter is on the left side 100nm
The right side, draw ratio is far more than 1000.Mainly by hexadecylamine as growth end-capping reagent, in conjunction with PVPK30's and CTAB
The preparation of ball chain shape copper nano-wire is realized in the effect of composite growth regulator.
2) the ball chain shape copper nano-wire is used in the preparation process of transparent conductive electrode, due to ball chain shape copper nano-wire phase
There is bigger contact area to linear copper nano-wire, show better light transmission rate and surface resistance, that is,
It says, is showed relative to linear copper nano-wire with better performance.
Detailed description of the invention
Fig. 1 a figure is the SEM photograph of ball chain shape copper nano-wire prepared by the present invention, and b figure is prepared by comparative example 1 of the present invention
The SEM photograph of product；
The light transmission rate under different area content of Fig. 2 ball chain shape copper nano-wire prepared by the present invention；
The light transmission rate and surface resistance composite diagram under different area content of Fig. 3 ball chain shape copper nano-wire prepared by the present invention.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
(hexadecane of 6.44g is added in the deionized water that the trisodium citrate of the copper sulphate of 5mM and 5mM is dissolved in 60mL in advance
Base amine), PVPK30 and the CTAB stirring of 0.2g is then added thereto, and the pH of mixed solution is adjusted to using sodium hydroxide
9；Later, which is placed in oil bath pan, the heating temperature that oil bath pan is arranged is 110 DEG C, after reaching the temperature, immediately
Reducing agent hydrazine hydrate is added into reaction mixture, is maintained at and reacts 8h at this temperature；After reaction, using isopropanol
Centrifuge washing is carried out to product with the mixed solution of n-hexane, the copper nano-wire of target product ball chain shape can be obtained.
Embodiment 2
(hexadecane of 6.44g is added in the deionized water that the trisodium citrate of the copper sulphate of 5mM and 5mM is dissolved in 60mL in advance
Base amine), PVPK30 and the CTAB stirring of 0.2g is then added thereto, and the pH of mixed solution is adjusted to using potassium hydroxide
10；Later, which is placed in oil bath pan, the heating temperature that oil bath pan is arranged is 115 DEG C, after reaching the temperature, is stood
Reducing agent sodium borohydride is added i.e. into reaction mixture, is maintained at and reacts 8h at this temperature；After reaction, use is different
The mixed solution of propyl alcohol and n-hexane carries out centrifuge washing to product, can obtain the copper nano-wire of target product ball chain shape.
Embodiment 3
(hexadecane of 6.44g is added in the deionized water that the trisodium citrate of the copper nitrate of 5mM and 5mM is dissolved in 60mL in advance
Base amine), PVPK30 and the CTAB stirring of 0.3g is then added thereto, and the pH of mixed solution is adjusted to using sodium hydroxide
10；Later, which is placed in oil bath pan, the heating temperature that oil bath pan is arranged is 120 DEG C, after reaching the temperature, is stood
Reducing agent hydrazine hydrate is added i.e. into reaction mixture, is maintained at and reacts 5h at this temperature；After reaction, using isopropyl
The mixed solution of pure and mild n-hexane carries out centrifuge washing to product, can obtain the copper nano-wire of target product ball chain shape.
Embodiment 4
(hexadecane of 6.44g is added in the deionized water that the trisodium citrate of the copper acetate of 5mM and 5mM is dissolved in 60mL in advance
Base amine), PVPK30 and the CTAB stirring of 0.3g is then added thereto, and the pH of mixed solution is adjusted to using potassium hydroxide
10；Later, which is placed in oil bath pan, the heating temperature that oil bath pan is arranged is 120 DEG C, after reaching the temperature, is stood
Reducing agent sodium borohydride is added i.e. into reaction mixture, is maintained at and reacts 5h at this temperature；After reaction, use is different
The mixed solution of propyl alcohol and n-hexane carries out centrifuge washing to product, can obtain the copper nano-wire of target product ball chain shape.
Embodiment 5
(hexadecane of 6.44g is added in the deionized water that the trisodium citrate of the copper sulphate of 5mM and 5mM is dissolved in 60mL in advance
Base amine), PVPK30 and the CTAB stirring of 0.2g is then added thereto, and the pH of mixed solution is adjusted to using sodium hydroxide
11；Later, which is placed in oil bath pan, the heating temperature that oil bath pan is arranged is 120 DEG C, after reaching the temperature, is stood
Reducing agent hydrazine hydrate is added i.e. into reaction mixture, is maintained at and reacts 5h at this temperature；After reaction, using isopropyl
The mixed solution of pure and mild n-hexane carries out centrifuge washing to product, can obtain the copper nano-wire of target product ball chain shape.
Comparative example 1
Other conditions are same as Example 1, and difference, which is only that, does not use PVPK30 and CTAB to cook growth regulator.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
Claims (9)
1. a kind of preparation method of the copper nano-wire of ball chain shape, which comprises the following steps:
Step 1: in deionized water by mantoquita dissolution, the trisodium citrate of equimolar amounts is then added thereto again, stirring is equal
It is even；
Step 2: the pH value of solution in step 1 being adjusted to 9-11, suitable growth regulator is then added and is mixed；
Step 3: the solution in step 2 being placed in oil bath pan, and so that oil bath pan is heated reaction system to certain temperature and carries out instead
It answers；
Step 4: after the temperature of water-bath reaches set temperature, then suitable reducing agent being added into reaction system, and maintain
5-8h is reacted at such a temperature；After reaction, carrying out centrifuge washing to it can be obtained the copper nano-wire of product ball chain shape.
2. a kind of preparation method of the copper nano-wire of ball chain shape according to claim 1, which is characterized in that step 1 is gone
Hexadecylamine is also added in ionized water in advance as growth end-capping reagent.
3. a kind of preparation method of the copper nano-wire of ball chain shape according to claim 1, which is characterized in that in step 1
Mantoquita refers to one of copper sulphate, copper nitrate, copper acetate or copper chloride.
4. a kind of preparation method of the copper nano-wire of ball chain shape according to claim 1, which is characterized in that pH in step 2
Regulator is one or more of sodium hydroxide, potassium hydroxide or calcium hydroxide.
5. a kind of preparation method of the copper nano-wire of ball chain shape according to claim 1, which is characterized in that raw in step 2
Long regulator refers to PVPK30 and CTAB.
6. a kind of preparation method of the copper nano-wire of ball chain shape according to claim 1, which is characterized in that one in step 3
Determine temperature and refers to 110-120 DEG C.
7. a kind of preparation method of the copper nano-wire of ball chain shape according to claim 1, which is characterized in that institute in step 4
Reducing agent refers to or mixtures thereof sodium borohydride, hydrazine hydrate.
8. the copper nano-wire of preparation method preparation according to claim 1-7, and it is applied to electrically conducting transparent
The application of electrode.
9. application according to claim 8, which is characterized in that prepare transparent conductive electrode using Meyer stick.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI793635B (en) * | 2020-06-15 | 2023-02-21 | 德克薩斯農工大學系統 | Copper nanowires and their use in plastics to improve thermal and electrical conductivity |
| CN115739110A (en) * | 2022-11-04 | 2023-03-07 | 湖州美奇医疗器械有限公司 | Preparation method and application of platinum-based catalyst |
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| 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 |
| CN109622987A (en) * | 2019-02-13 | 2019-04-16 | 济南大学 | The method that one-step method prepares the copper nano-wire of the polypyrrole package of core-shell structure |
| CN110070957A (en) * | 2019-03-26 | 2019-07-30 | 天津大学 | High optical transmission and the flexible metal nano thin-film of electric conductivity and preparation method thereof |
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2019
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| CN102792385A (en) * | 2009-12-07 | 2012-11-21 | 杜克大学 | Compositions and methods for growing copper nanowires |
| CN108526480A (en) * | 2018-03-16 | 2018-09-14 | 浙江大学 | A kind of method that low cost quickly prepares copper nano-wire |
| CN108470603A (en) * | 2018-04-23 | 2018-08-31 | 天津大学 | A kind of preparation method of copper nano-wire transparent electrode |
| CN109622987A (en) * | 2019-02-13 | 2019-04-16 | 济南大学 | The method that one-step method prepares the copper nano-wire of the polypyrrole package of core-shell structure |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI793635B (en) * | 2020-06-15 | 2023-02-21 | 德克薩斯農工大學系統 | Copper nanowires and their use in plastics to improve thermal and electrical conductivity |
| CN115739110A (en) * | 2022-11-04 | 2023-03-07 | 湖州美奇医疗器械有限公司 | Preparation method and application of platinum-based catalyst |
| CN115739110B (en) * | 2022-11-04 | 2024-01-30 | 湖州美奇医疗器械有限公司 | Preparation method and application of platinum-based catalyst |
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Application publication date: 20191112 |