CN1727523A - The method of liquid phase synthesizing one-dimensional super long Nano line of metal copper - Google Patents
The method of liquid phase synthesizing one-dimensional super long Nano line of metal copper Download PDFInfo
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- CN1727523A CN1727523A CN 200410070765 CN200410070765A CN1727523A CN 1727523 A CN1727523 A CN 1727523A CN 200410070765 CN200410070765 CN 200410070765 CN 200410070765 A CN200410070765 A CN 200410070765A CN 1727523 A CN1727523 A CN 1727523A
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Abstract
The present invention relates to the method for the synthetic super long Nano line of metal copper of a kind of liquid phase, comprise taking by weighing the divalent metal mantoquita, put into the container that has agitating function, add a certain amount of pure water, its concentration is within the 0.001-0.1M scope; Mol ratio by cupric ion and alkylamine is Cu
2+: RNH
2=1: 1-1: 10; The aliphatic alkylamine that takes by weighing adds to stir in the above-mentioned aqueous solution that is dissolved with cupric ion and forms even milk sap; In the milk sap charged pressure container that obtains, be warming up to 100-200 ℃ of temperature, carried out hydro-thermal reaction in constant temperature 4-72 hour after; Naturally cool to room temperature; Reaction finishes after repeatedly washing, and filtering and obtaining diameter is 10-500nm, and maximum length-to-diameter ratio can reach 10
6, super long Nano line of metal copper.Present method raw material is cheap, only needs a step hydro-thermal reaction can obtain product.This method prepares the diameter and the length-to-diameter ratio of copper nano-wire and can be regulated and control by the control reaction conditions.
Description
Technical field
The invention belongs to preparation of nanomaterials, the method for the extensive synthesizing one-dimensional super long Nano line of metal copper of particularly a kind of liquid phase.
Background technology
Metal nanometer line is because its unique physical properties and quantum size effect, be expected to field of nanometer technology as: the manufacture view of nanoelectronic, photoelectricity, magnetics device plays an important role, and has set up possible model for the relation between research electron transport, optics and other physical phenomenons (as: quantum conduction and small-size effect) and material intrinsic structure, dimension and the size.So synthetic, sign and performance study to metal nanometer line over past ten years receive much attention.Because the metallic copper of body material has good heat, electrical conductivity, also be in all metals, to use maximum materials as connecting lead.Copper nano-wire may be widely used in the receiving of future, microelectronics technology, has great potential using value.So in recent years, Many researchers has produced keen interest to the research (comprising preparation, sign and physical properties test) of Nano line of metal copper.Yet for the copper nano-wire that is expected to widespread use, preparation is the principal element (as: quality, cost and productive rate and size control, length-to-diameter ratio control) of its development of restriction.This is because the method for the synthetic Nano line of metal copper of preparation all has more shortcoming at present, as the needs specific installation, or severe reaction conditions, or productive rate is low, or complex process or the like, all be not suitable for industrialization, large-scale production.Mainly be listed below:
Template method: this method is to utilize nanoporous or mesoporous material (as carbon nanotube, mesoporous SiO
2, polymkeric substance or electrochemical anodic oxidation aluminum oxide) be template, by electrochemical deposition or utilize the copper compound in the reductive agent reduction template duct to obtain copper nano-wire; As document 1: " advanced material " (" Adv.Mater.〉2001; 13; 62 is described; though this method can come controlledly synthesis to go out the copper nano-wire of homogeneous by the diameter and the template thickness in change template duct; but need remove template with thermal treatment or dissolution with solvents way usually; complex process, and productive rate is relatively low, is not suitable for industrialization, large-scale production.
Physical method: the Liu Zongwen of Japanese national Materials science institute in 2003 etc. have developed the method that a kind of single stage method prepares copper nano-wire, as document 2: " advanced material " (" Adv.Mater. " 2003,15,303) described, be called vacuum gas evaporation method: comprise producing copper steam, sedimentary again process in substrate then under the condition of low pressure or vacuum.Though the product copper nano-wire better crystallinity degree that this method obtains, productive rate is also higher, and the length-to-diameter ratio of products therefrom is wayward, and purity is lower, and prior shortcoming is that preparation process needs specific installation, the condition harshness.
Chemical process: there are two kinds, a kind of solid phase reduction method that is based on gas-solid reaction growth (VSRG) mechanism, as document 3: " advanced material " (" Adv.Mater. " 2003,15,235) is described: with (Me
3Si)
4Si the sealing reaction tubes in 300 ℃ the reduction CuCl
2Obtain the 1-dimention nano copper product.The product that obtains is copper nanometer rod and nano wire, and is not easily separated, if will obtain the single thing of copper nano-wire, reactant should be high-purity CuCl (99.99%), and also need add deep fat (PDMS) in the reaction system.This method cost height, reaction conditions are also relatively harsher, are unsuitable for large-scale production.
Another kind is a liquid phase reduction: promptly reduce copper compound at the soln using reductive agent.Compare with aforementioned solid phase method (comprising physical method and chemical process), these class methods flexibly, effectively, easy control of reaction conditions and method that can the large-scale production copper nano-wire.Though occurred the method with the synthetic Nano line of metal copper of solution method in 2003, as document 4: " physical chemistry magazine B " (" J.Phys.Chem.B " 2003,107,12658-12661) described, raw materials used is CuSO
45H
2O, glycerol, NaOH, H
3PO
3And Sodium dodecylbenzene sulfonate, in encloses container, heat up reduction reaction takes place, synthetic Nano line of metal copper.Though this method productive rate is higher, complex synthetic route, raw materials cost is also higher, is unsuitable for large-scale production.
Summary of the invention
The objective of the invention is to solve existing at present synthetic metal nano line method cost height, implementation condition harshness, complex process or the lower shortcoming of productive rate; A kind of raw materials cost that adopts is cheap, technology is simple, reaction conditions is gentle thereby provide, and the high liquid phase of one dimension, overlength copper nano-wire controllable size, purity of the preparation method of synthetic Nano line of metal copper on a large scale.
The objective of the invention is to realize by the following technical solutions:
Super long Nano line of metal copper synthetic method provided by the invention may further comprise the steps:
(1). take by weighing the divalent metal mantoquita, described divalent metal mantoquita comprises CuCl
2Or CuSO
4Put into the container that has agitating function, add a certain amount of pure water, stirring and dissolving; The pure water amount that is added by the cupric ion concentration of aqueous solution within the 0.001-0.1M scope;
(2). taking by weighing aliphatic alkylamine then, is Cu by the mol ratio of cupric ion and alkylamine
2+: RNH
2=1: 1-1: 10; The aliphatic alkylamine that takes by weighing is added in the above-mentioned aqueous solution that is dissolved with cupric ion, and fully stir and form even milk sap, till aliphatic alkylamine dissolves fully;
(3) hydro-thermal is synthetic: with the milk sap that step (2) obtains, be that 70%-90% is packed in the pressurized vessel, after the sealing, be warming up to 100-200 ℃ of temperature by compactedness, carried out hydro-thermal reaction in constant temperature 4-72 hour after; Naturally cool to room temperature;
(4) product that step (3) is obtained separates: remove supernatant liquid after the centrifugation, lower floor's solid product is used deionized water respectively successively, and normal hexane and absolute ethanol washing promptly get the product copper nano-wire more than three times.
Also comprise step (5) vacuum-drying: in room temperature, 10
-3Promptly got the product copper nano-wire under the normal atmosphere in vacuum-drying 1-4 hour.
Described aliphatic alkylamine is meant that carbonatoms is 8 to 18 alkylamine.
The described container that has agitating function comprises: the container of electronic stirring or magnetic agitation
The Nano line of metal copper that aforesaid method synthesizes, diameter are 10-500nm, and maximum length-to-diameter ratio can reach 10
6This method prepares the diameter of copper nano-wire and length-to-diameter ratio can be by the control reaction conditions: temperature of reaction, initial reactant mol ratio and reaction times are regulated and control, for example: the diameter that can reach the regulation and control Nano line of metal copper by control reaction temperature; And for example can reach the diameter of regulation and control Nano line of metal copper by control initial reactant mol ratio; Can also can reach the length-to-diameter ratio of regulation and control Nano line of metal copper by controlling reaction time.
Super long Nano line of metal copper provided by the invention can be used to study quantum confinement, dimensional effect, the electrons transport property of copper nano-wire, for the relation of studying between other physical phenomenons, character and the copper nano-wire essential structure provides model.The more important thing is with good conductive, the heat conductivility of body material and compare, be expected to be widely used in microelectronics and field of nanometer devices.
The invention has the advantages that: synthetic method of the present invention is very simple, only needs a step hydro-thermal reaction can obtain super long Nano line of metal copper, the Nano line of metal copper that synthesizes, and diameter is 10-500nm, maximum length-to-diameter ratio can reach 10
6Raw materials used cheapness only needs divalent metal mantoquita (as: CuCl
2, CuSO
4) with carbonatoms be the aliphatic alkylamine of 8-18, without any need for organic solvent and other tensio-active agents; Synthesis technique is quite simple, and required plant and instrument all is common chemical industry equipment commonly used, and cost is low, good reproducibility.This method prepares the diameter of copper nano-wire and length-to-diameter ratio can be by the control reaction conditions: temperature of reaction, initial reactant mol ratio and reaction times are regulated and control, the prepared product purity height that goes out, length-to-diameter ratio is big, and steady quality, is suitable for large-scale industrialization production.
Description of drawings
The field emission electron microstructure of the overlength copper nano-wire that Fig. 1 liquid-phase synthesis process of the present invention obtains.
The field emission electron microstructure of the low magnification copper nano-wire of the overlength copper nano-wire that Fig. 2 liquid-phase synthesis process of the present invention obtains.
The field emission electron microstructure of the high-amplification-factor copper nano-wire of the overlength copper nano-wire that Fig. 3 liquid-phase synthesis process of the present invention obtains.
The size control of the overlength copper nano-wire that Fig. 4 liquid-phase synthesis process of the present invention obtains is the field emission electron microstructure of the copper nano-wire of (50nm) very evenly.
Embodiment:
Embodiment 1: the CuCl that takes by weighing 0.001mol
22H
2O adds 100ml distilled water in the reactor that band stirs, stirring and dissolving adds 0.001mol stearylamine (C then
18H
37NH
2), fully stir until forming even blue milk sap, there is not undissolved stearylamine.Gained liquid is changed in the molten bullet of stainless steel pressure, and compactedness is 85%, and sealing covers completely, be warming up to 120 ℃ and kept 72 hours, naturally cool to room temperature then, collect the gained solid product after the centrifugation, with dehydrated alcohol, normal hexane and deionized water wash more than three times, in room temperature, 10
-3Vacuum-drying is 1 hour under the normal atmosphere, vacuum-drying, and promptly getting the product mean diameter is that 50nm, length can reach 10
-3The copper nano-wire of rice.
Embodiment 2: the CuCl that takes by weighing 0.001mol
22H
2O adds 75ml distilled water in the reactor that band stirs, stirring and dissolving adds 0.002mol stearylamine (C then
18H
37NH
2), fully stir until forming even blue milk sap, there is not undissolved stearylamine.Gained liquid is changed in the molten bullet of stainless steel pressure, and compactedness is 80%, and sealing covers completely, be warming up to 160 ℃ and kept 50 hours, naturally cool to room temperature then, collect products obtained therefrom after the centrifugation, with dehydrated alcohol, normal hexane and deionized water wash more than three times, in room temperature, 10
-3Vacuum-drying is 4 hours under the normal atmosphere, vacuum-drying, and promptly getting the product mean diameter is that 150nm, length can reach 10
-2The copper nano-wire of rice.
Embodiment 3: the CuCl that takes by weighing 0.002mol
22H
2O adds 75ml distilled water in the reactor that band stirs, stirring and dissolving adds 0.004mol stearylamine (C then
18H
37NH
2), fully stir until forming even blue milk sap, there is not undissolved stearylamine.Gained liquid is changed in the molten bullet of stainless steel pressure, and compactedness is 65%, and sealing covers completely, be warming up to 200 ℃ and kept 20 hours, naturally cool to room temperature then, collect products obtained therefrom after the centrifugation, with dehydrated alcohol, normal hexane and deionized water wash more than three times, in room temperature, 10
-3Vacuum-drying is 3 hours under the normal atmosphere, vacuum-drying, and promptly getting the product mean diameter is that 10nm, length can reach 10
-2The copper nano-wire of rice.
Embodiment 4: the CuCl that takes by weighing 0.01mol
22H
2O adds 100ml distilled water in the reactor that band stirs, stirring and dissolving adds 0.05mol n-octyl amine (C then
8H
17NH
2), fully stir until forming even blue milk sap, there is not undissolved n-octyl amine.Gained liquid is changed in the molten bullet of stainless steel pressure, and compactedness is 95%, and sealing covers completely, be warming up to 100 ℃ and kept 20 hours, naturally cool to room temperature then, collect products obtained therefrom after the centrifugation, with dehydrated alcohol, normal hexane and deionized water wash more than three times, in room temperature, 10
-3Vacuum-drying is 2 hours under the normal atmosphere, and vacuum-drying promptly gets product diameter average out to 500nm, length can reach 10
-3The copper nano-wire of rice.
Embodiment 5: the CuCl that takes by weighing 0.0001mol
22H
2O adds 100ml distilled water in the reactor that band stirs, stirring and dissolving adds 0.001mol stearylamine (C then
18H
37NH
2), fully stir until forming even blue milk sap, there is not undissolved stearylamine.Gained liquid is changed in the molten bullet of stainless steel pressure, and compactedness is 90%, and sealing covers completely, be warming up to 120 ℃ and kept 40 hours, naturally cool to room temperature then, collect products obtained therefrom after the centrifugation, with dehydrated alcohol, normal hexane and deionized water wash more than three times, in 60 ℃ of temperature, 10
-3Vacuum-drying is 1.5 hours under the normal atmosphere, vacuum-drying, and promptly getting the product diameter is that 40nm, length can reach 10
-3The copper nano-wire of rice.
Embodiment 6: the CuSO that takes by weighing 0.002mol
45H
2O adds 75ml distilled water in the reactor that band stirs, stirring and dissolving adds 0.002mol cetylamine (C then
18H
37NH
2), fully stir until forming even blue milk sap, there is not undissolved cetylamine.Gained liquid is changed in the molten bullet of stainless steel pressure, and compactedness is 85%, and sealing covers completely, be warming up to 180 ℃ and kept 4 hours, naturally cool to room temperature then, collect products obtained therefrom after the centrifugation, with dehydrated alcohol, normal hexane and deionized water wash more than three times, in room temperature, 10
-3Vacuum-drying is 2.5 hours under the normal atmosphere, vacuum-drying, and promptly getting the product diameter is that 10nm, length can reach 10
-4The copper nano-wire of rice.
Claims (3)
1. the method for a liquid phase synthesizing one-dimensional super long Nano line of metal copper may further comprise the steps:
(1). take by weighing the divalent metal mantoquita, described divalent metal mantoquita comprises CuCl
2Or CuSO
4Put into the container that has agitating function, add a certain amount of pure water, stirring and dissolving; The pure water amount that is added by the cupric ion concentration of aqueous solution within the 0.001-0.1M scope;
(2). taking by weighing aliphatic alkylamine then, is Cu by the mol ratio of cupric ion and alkylamine
2+: RNH
2=1: 1-1: 10; The aliphatic alkylamine that takes by weighing is added in the above-mentioned aqueous solution that is dissolved with cupric ion, and fully stir and form even milk sap, till aliphatic alkylamine dissolves fully;
(3) hydro-thermal is synthetic: with the milk sap that step (2) obtains, be that 70%-90% is packed in the pressurized vessel by compactedness, cover sealing completely after, be warming up to 100-200 ℃ of temperature, carried out hydro-thermal reaction in constant temperature 4-72 hour after; Naturally cool to room temperature;
(4) product that step (3) is obtained separates: remove supernatant liquid after the centrifugation, lower floor's solid product is used deionized water respectively successively, and normal hexane and absolute ethanol washing promptly get the product copper nano-wire more than three times.
2. by the method for the described liquid phase synthesizing one-dimensional super long Nano line of metal copper of claim 1, it is characterized in that: also comprise step (5) vacuum-drying: under room temperature, 10-3 normal atmosphere, promptly got the product copper nano-wire in vacuum-drying 1-4 hour.
3. by the method for the described liquid phase synthesizing one-dimensional super long Nano line of metal copper of claim 1, it is characterized in that: described aliphatic alkylamine is meant that carbonatoms is 8 to 18 alkylamine.
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| CN101161380B (en) * | 2006-10-10 | 2012-01-04 | 三星电机株式会社 | Method for manufacturing copper nanoparticles and copper nanoparticles manufactured using the same |
| CN101319357B (en) * | 2008-06-20 | 2012-04-04 | 江苏大学 | Preparation of copper nano-wire with microwave auxiliary liquid phase reduction |
| WO2012094072A1 (en) * | 2011-01-04 | 2012-07-12 | Carestream Health, Inc. | Nanowire recovery methods, compositions, and articles |
| CN102601382A (en) * | 2012-03-27 | 2012-07-25 | 苏州冷石纳米材料科技有限公司 | Method for massively preparing overlength copper nanowires |
| CN102787347A (en) * | 2012-09-04 | 2012-11-21 | 上海师范大学 | Preparation method of overlong copper nanowire and conductive copper nanowire film |
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| CN104162657A (en) * | 2014-07-21 | 2014-11-26 | 江苏大学 | Super-long copper nanowire and preparing method thereof |
| CN104959622A (en) * | 2015-06-09 | 2015-10-07 | 重庆文理学院 | Synthesis method for copper nanowire with different length-diameter ratios |
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2004
- 2004-07-26 CN CN 200410070765 patent/CN1283851C/en not_active Expired - Lifetime
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| CN101161380B (en) * | 2006-10-10 | 2012-01-04 | 三星电机株式会社 | Method for manufacturing copper nanoparticles and copper nanoparticles manufactured using the same |
| CN101319357B (en) * | 2008-06-20 | 2012-04-04 | 江苏大学 | Preparation of copper nano-wire with microwave auxiliary liquid phase reduction |
| US20130084238A1 (en) * | 2010-05-12 | 2013-04-04 | Unist Academy-Industry Research Corporation | Method of making nanomaterial and method of fabricating secondary battery using the same |
| WO2012094072A1 (en) * | 2011-01-04 | 2012-07-12 | Carestream Health, Inc. | Nanowire recovery methods, compositions, and articles |
| US8696947B2 (en) | 2011-01-04 | 2014-04-15 | Carestream Health, Inc. | Nanowire recovery methods, compositions, and articles |
| CN102601382A (en) * | 2012-03-27 | 2012-07-25 | 苏州冷石纳米材料科技有限公司 | Method for massively preparing overlength copper nanowires |
| CN102601382B (en) * | 2012-03-27 | 2014-04-02 | 苏州冷石纳米材料科技有限公司 | Method for massively preparing overlength copper nanowires |
| CN102787347B (en) * | 2012-09-04 | 2015-10-21 | 上海师范大学 | The preparation method of a kind of super long copper nano wire and copper nano-wire conductive film |
| CN102787347A (en) * | 2012-09-04 | 2012-11-21 | 上海师范大学 | Preparation method of overlong copper nanowire and conductive copper nanowire film |
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| CN103498198B (en) * | 2013-10-24 | 2016-03-23 | 南京信息工程大学 | A kind of preparation method of positive pentagonal prism shape copper micro wire |
| CN103498198A (en) * | 2013-10-24 | 2014-01-08 | 南京信息工程大学 | Preparation method of regular pentagonal prism-shaped copper micrometer wire |
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| CN104162657A (en) * | 2014-07-21 | 2014-11-26 | 江苏大学 | Super-long copper nanowire and preparing method thereof |
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| CN104162680B (en) * | 2014-07-28 | 2016-06-29 | 江苏大学 | A kind of method of continuous synthesis copper nano-wire |
| CN104959622A (en) * | 2015-06-09 | 2015-10-07 | 重庆文理学院 | Synthesis method for copper nanowire with different length-diameter ratios |
| CN105170994A (en) * | 2015-09-17 | 2015-12-23 | 浙江工业大学 | Solvothermal method for preparing copper nanowires |
| CN105328206A (en) * | 2015-11-19 | 2016-02-17 | 北京化工大学 | Method for preparing copper nanowires through oil-phase chemical reduction |
| CN106493391A (en) * | 2016-12-12 | 2017-03-15 | 中国科学技术大学 | A kind of method of purification of copper nano-wire |
| CN109420772A (en) * | 2017-08-25 | 2019-03-05 | Tcl集团股份有限公司 | Hud typed Cu/SnO2Nano wire, preparation method and application |
| CN109560256A (en) * | 2018-11-29 | 2019-04-02 | 西交利物浦大学 | The preparation method and applications of copper silicon composite cathode piece |
| US20210388180A1 (en) * | 2020-06-15 | 2021-12-16 | The Texas A&M University System | Copper nanowires and their use in plastics to improve thermal and electrical conductivity |
| CN113263185A (en) * | 2021-05-08 | 2021-08-17 | 延边大学 | Method for preparing bent copper nanowires by using secondary addition method of polyhydric alcohol |
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