CN106424750A - Preparation method for multi-dimensional copper nanowire material - Google Patents
Preparation method for multi-dimensional copper nanowire material Download PDFInfo
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- CN106424750A CN106424750A CN201610837753.7A CN201610837753A CN106424750A CN 106424750 A CN106424750 A CN 106424750A CN 201610837753 A CN201610837753 A CN 201610837753A CN 106424750 A CN106424750 A CN 106424750A
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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
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses a preparation method for a multi-dimensional copper nanowire material. The preparation method for the multi-dimensional copper nanowire material comprises the following steps that (1) with a metallic copper material as a precursor, a multi-dimensional cuprous oxide nanowire is obtained through calcination in air, wherein the calcination temperature is 200-800 DEG C, and the calcination time is 0.5-12 hours; and (2) the multi-dimensional cuprous oxide nanowire is reduced through an electrochemical reduction method or a chemical reduction method, and thus a metallic copper nanowire is obtained. According to the preparation method for the multi-dimensional copper nanowire material, cuprous oxide nanowires of different forms can be obtained by controlling the temperature and the calcination time, and the metallic copper nanowires with different catalytic activities can be prepared through different reduction methods; the preparation technique is simple, a large-scale volume production mode can be formed easily, and the cost is reduced greatly; and the length of the produced copper nanowire is 5-60 [mu]m, and the diameter of the produced copper nanowire is 50-100 nm.
Description
【Technical field】
The invention belongs to Nanometer Copper manufacturing technology field, more particularly to a kind of preparation side of multidimensional copper nano-wire material
Method.
【Background technology】
Copper nano-wire has higher electrical conductivity, has potential at aspects such as microelectronic component, chemistry or biology sensors
Application prospect, cause and widely pay close attention to both at home and abroad.Nanometer Copper has superplastic extensibility, more than 50 times can be elongated at room temperature and
Occur without crackle, as a kind of new nanostructured NANO CRYSTAL COPPER WIRE film, ITO (tin-doped indium oxide) can be replaced thin
Film, can substantially reduce the manufacturing cost of the displays such as mobile phone, electronic reader and iPad, therefore cause increasing people's research
Preparation method with regard to copper nano-wire.
A kind of nano cuprous oxide wire porous is disclosed thin in prior art Patent Application No. 201410014003.0
Film and its preparation method and application, with cuprous thiocyanate membrane as precursor, can prepare nano cuprous oxide wire porous membrane;Specially
A kind of nano cuprous oxide wire material and its simple method for preparing is disclosed, ultrasonic in sharp Application No. 201410018809.7
Under ripple effect, cuprous sulfocyanide powder can also prepare nano cuprous oxide wire material with aqueous slkali reaction.Research afterwards is sent out
Existing, number of patent application is to disclose a kind of preparation method of nano cuprous oxide wire material in 201410031465.3, if adopted
With relatively dense aqueous slkali, even without ultrasonic wave it is also possible to make cuprous sulfocyanide powder be transformed into nano cuprous oxide wire
Material.Above method process is relative complex, and material therefor is expensive, and cuprous oxide reactivity is several for metallic copper
There is no catalytic reaction activity.And cannot be carried out producing in batches on a large scale, lead to the product price manufacturing higher.
Therefore, it is necessary to provide a kind of preparation method of new multidimensional copper nano-wire material to solve the above problems.
【Content of the invention】
Present invention is primarily targeted at providing a kind of preparation method of multidimensional copper nano-wire material, its process is simple, and
It is capable of producing in batches, reduce cost.
The present invention is achieved through the following technical solutions above-mentioned purpose:A kind of preparation method of multidimensional copper nano-wire material, bag
Include following steps,
1) with metal copper material as precursor, in atmosphere multidimensional nano cuprous oxide wire, roast temperature are obtained by roast
Spend for 200~800 DEG C, calcination times are 0.5~12 hour;
2) pass through electrochemical reduction or the reduction of described multidimensional nano cuprous oxide wire is obtained gold by the method for electronation
Belong to copper nano-wire.
Further, described precursor can be using copper materials such as copper mesh, copper sheet or metallic copper foams.
Further, the operating procedure of described electrochemical reduction includes,
1) described multidimensional nano cuprous oxide wire is set to working electrode;
2) graphite or platinum are as to electrode;
3) silver/silver chlorate is as reference electrode;
4), as electrolyte, biasing voltage controls in -0.3~0.8V, until all described for sodium sulphate or other salting liquids
Multidimensional nano cuprous oxide wire is reduced into described Nano line of metal copper.
Further, the operating procedure of described electronation includes training described multidimensional nano cuprous oxide wire in hydrogen
Burn, firing temperature controls at 100~300 DEG C, calcination times 0.5~3 hour, until all described multidimensional nano cuprous oxide wires
It is reduced into described Nano line of metal copper.
Compared with prior art, the having the beneficial effects that of the preparation method of a kind of multidimensional of present invention copper nano-wire material:Logical
Cross and control temperature and calcination times to produce the nano cuprous oxide wire of different shape;Can be prepared into not by different reduction modes
Nano line of metal copper with catalysis activity;Preparation process is simple of the present invention, easily forms large-scale batch production pattern, significantly drops
Low cost.The length of the copper nano-wire produced by the preparation method of the present invention is 5~60um, a diameter of 50~100nm.
【Brief description】
Fig. 1 is the low resolution SEM image for the copper nano-wire going out for the present invention;
The high-resolution SEM image of the copper nano-wire that Fig. 2 prepares for the present invention.
【Specific embodiment】
Embodiment one
The present embodiment is the preparation method of multidimensional copper nano-wire material, and it comprises the following steps:
1) with metal copper material as precursor, such as copper mesh, copper sheet or metallic copper foam etc., obtained by roast in atmosphere
Multidimensional nano cuprous oxide wire, firing temperature is 200 DEG C, and calcination times are 0.5 hour;
2) multidimensional nano cuprous oxide wire is set to working electrode, as to electrode, silver/silver chlorate is as ginseng for graphite or platinum
Ratio electrode (or other similar reference electrodes), sodium sulphate or other salting liquids as electrolyte, biasing voltage controls -0.3~
0.8V, until all nano cuprous oxide wires are reduced into Nano line of metal copper.
In the present embodiment, precursor material is preferably metallic copper foam.
Embodiment two
The present embodiment is the preparation method of multidimensional copper nano-wire material, and it comprises the following steps:
1) with metal copper material as precursor, such as copper mesh, copper sheet or metallic copper foam etc., obtained by roast in atmosphere
Multidimensional nano cuprous oxide wire, firing temperature is 200 DEG C, and calcination times are 8 hours;
2) by multidimensional nano cuprous oxide wire in hydrogen roast, firing temperature controls at 100~300 DEG C, calcination times
0.5~3 hour, until all nano cuprous oxide wires are reduced into Nano line of metal copper.
In the present embodiment, precursor material is preferably metallic copper foam.
Embodiment three
The present embodiment is the preparation method of multidimensional copper nano-wire material, and it comprises the following steps:
1) with metal copper material as precursor, such as copper mesh, copper sheet or metallic copper foam etc., obtained by roast in atmosphere
Multidimensional nano cuprous oxide wire, firing temperature is 200 DEG C, and calcination times are 12 hours;
2) multidimensional nano cuprous oxide wire is set to working electrode, as to electrode, silver/silver chlorate is as ginseng for graphite or platinum
Ratio electrode (or other similar reference electrodes), sodium sulphate or other salting liquids as electrolyte, biasing voltage controls -0.3~
0.8V, until all nano cuprous oxide wires are reduced into Nano line of metal copper.
In the present embodiment, precursor material is preferably metallic copper foam.
Example IV
The present embodiment is the preparation method of multidimensional copper nano-wire material, and it comprises the following steps:
1) with metal copper material as precursor, such as copper mesh, copper sheet or metallic copper foam etc., obtained by roast in atmosphere
Multidimensional nano cuprous oxide wire, firing temperature is 600 DEG C, and calcination times are 0.5 hour;
2) by multidimensional nano cuprous oxide wire in hydrogen roast, firing temperature controls at 100~300 DEG C, calcination times
0.5~3 hour, until all nano cuprous oxide wires are reduced into Nano line of metal copper.
In the present embodiment, precursor material is preferably metallic copper foam.
Embodiment five
The present embodiment is the preparation method of multidimensional copper nano-wire material, and it comprises the following steps:
1) with metal copper material as precursor, such as copper mesh, copper sheet or metallic copper foam etc., obtained by roast in atmosphere
Multidimensional nano cuprous oxide wire, firing temperature is 600 DEG C, and calcination times are 8 hours;
2) multidimensional nano cuprous oxide wire is set to working electrode, as to electrode, silver/silver chlorate is as ginseng for graphite or platinum
Ratio electrode (or other similar reference electrodes), sodium sulphate or other salting liquids as electrolyte, biasing voltage controls -0.3~
0.8V, until all nano cuprous oxide wires are reduced into Nano line of metal copper.
In the present embodiment, precursor material is preferably metallic copper foam.
As accompanying drawing 1,2 show the low resolution of the copper nano-wire that the present embodiment is obtained and high-resolution SEM image.
Embodiment six
The present embodiment is the preparation method of multidimensional copper nano-wire material, and it comprises the following steps:
1) with metal copper material as precursor, such as copper mesh, copper sheet or metallic copper foam etc., obtained by roast in atmosphere
Multidimensional nano cuprous oxide wire, firing temperature is 600 DEG C, and calcination times are 12 hours;
2) by multidimensional nano cuprous oxide wire in hydrogen roast, firing temperature controls at 100~300 DEG C, calcination times
0.5~3 hour, until all nano cuprous oxide wires are reduced into Nano line of metal copper.
In the present embodiment, precursor material is preferably metallic copper foam.
Embodiment seven
The present embodiment is the preparation method of multidimensional copper nano-wire material, and it comprises the following steps:
1) with metal copper material as precursor, such as copper mesh, copper sheet or metallic copper foam etc., obtained by roast in atmosphere
Multidimensional nano cuprous oxide wire, firing temperature is 800 DEG C, and calcination times are 8 hours;
2) multidimensional nano cuprous oxide wire is set to working electrode, as to electrode, silver/silver chlorate is as ginseng for graphite or platinum
Ratio electrode (or other similar reference electrodes), sodium sulphate or other salting liquids as electrolyte, biasing voltage controls -0.3~
0.8V, until all nano cuprous oxide wires are reduced into Nano line of metal copper.
In the present embodiment, precursor material is preferably metallic copper foam.
Embodiment eight
The present embodiment is the preparation method of multidimensional copper nano-wire material, and it comprises the following steps:
1) with metal copper material as precursor, such as copper mesh, copper sheet or metallic copper foam etc., obtained by roast in atmosphere
Multidimensional nano cuprous oxide wire, firing temperature is 800 DEG C, and calcination times are 12 hours;
2) by multidimensional nano cuprous oxide wire in hydrogen roast, firing temperature controls at 100~300 DEG C, calcination times
0.5~3 hour, until all nano cuprous oxide wires are reduced into Nano line of metal copper.
In the present embodiment, precursor material is preferably metallic copper foam.
The preparation method of multidimensional copper nano-wire material of the present invention is passed through to control temperature and calcination times to produce different shape
Nano cuprous oxide wire;The Nano line of metal copper of different catalytically active can be prepared into by different reduction modes;System of the present invention
Standby process is simple, easily forms large-scale batch production pattern, greatly reduces cost.Produced by the preparation method of the present invention
The length of the copper nano-wire going out is 5~60um, a diameter of 50~100nm.
Above-described is only some embodiments of the present invention.For the person of ordinary skill of the art, not
On the premise of departing from the invention design, some deformation can also be made and improve, these broadly fall into the protection model of the present invention
Enclose.
Claims (4)
1. a kind of preparation method of multidimensional copper nano-wire material it is characterised in that:Comprise the following steps,
1) with metal copper material as precursor, in atmosphere multidimensional nano cuprous oxide wire is obtained by roast, firing temperature is
200~800 DEG C, calcination times are 0.5~12 hour;
2) pass through electrochemical reduction or the reduction of described multidimensional nano cuprous oxide wire is obtained metallic copper by the method for electronation
Nano wire.
2. multidimensional copper nano-wire material as claimed in claim 1 preparation method it is characterised in that:Described precursor can adopt copper
Net, copper sheet or metallic copper foam or other copper materials.
3. multidimensional copper nano-wire material as claimed in claim 1 preparation method it is characterised in that:Described electrochemical reduction
Operating procedure includes,
1) described multidimensional nano cuprous oxide wire is set to working electrode;
2) graphite or platinum are as to electrode;
3) silver/silver chlorate is as reference electrode;
4) as electrolyte, biasing voltage controls in -0.3~0.8V, until all described multidimensional for sodium sulphate or other salting liquids
Nano cuprous oxide wire is reduced into described Nano line of metal copper.
4. multidimensional copper nano-wire material as claimed in claim 1 preparation method it is characterised in that:The behaviour of described electronation
Include described multidimensional nano cuprous oxide wire roast in hydrogen as step, firing temperature controls at 100~300 DEG C, roast
0.5~3 hour time, until all described multidimensional nano cuprous oxide wires are reduced into described Nano line of metal copper.
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Cited By (5)
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CN108570710A (en) * | 2018-05-16 | 2018-09-25 | 中国科学院上海微系统与信息技术研究所 | The preparation method of copper whisker |
CN109267117A (en) * | 2018-09-27 | 2019-01-25 | 安庆北化大科技园有限公司 | A kind of electrode material and preparation method thereof of multi-stage nano composite construction |
CN109881220A (en) * | 2019-02-14 | 2019-06-14 | 安庆北化大科技园有限公司 | Method, conducting base composite material and the application of conducting base growth copper nanometer sheet |
CN110302808A (en) * | 2018-12-28 | 2019-10-08 | 江南大学 | A kind of rodlike molybdenum disulfide/copper sulphide nano composite material and preparation method |
CN115287765A (en) * | 2022-07-11 | 2022-11-04 | 大连理工大学 | Single crystal copper oxide nanowire and simple preparation method of copper nanowire |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN109267117A (en) * | 2018-09-27 | 2019-01-25 | 安庆北化大科技园有限公司 | A kind of electrode material and preparation method thereof of multi-stage nano composite construction |
CN110302808A (en) * | 2018-12-28 | 2019-10-08 | 江南大学 | A kind of rodlike molybdenum disulfide/copper sulphide nano composite material and preparation method |
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