CN105562709A - Preparation method for superfine copper nano particles - Google Patents
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Abstract
The invention provides a method for preparing superfine copper nano particles by utilizing immiscible liquid-liquid two-phase interface reaction. The method comprises the following steps of firstly, dissolving a copper salt into a non-polar solvent to prepare a copper-containing source solution or dissolving a copper salt into a non-polar solvent and then emulsifying witha polar solvent to prepare a copper-containing source solution, and dissolving a reducing agent into the polar solvent to prepare a reducing solution; forming an immiscible two-phase system by the reducing solution and the copper-containing source solution, thereby obtaining a stable liquid-liquid interface; and at certain temperature, reacting at the liquid-liquid interface to generate the superfine copper nano particles. The method can be used for preparing the superfine copper nano particles with particle diameters smaller than 10 nanometers, and the superfine copper nano particles have fewer impurities, pure components, good crystallization quality, and uniform sizes and morphology, can be stably dispersed into the immiscible two-phase system obtained by reaction without surface modifying and coating, and can standfor a long time in normal-temperature air without being oxidized. The method is simple, is low in energy consumption, is low in cost, is easy to control, and is high in practicability, and can be used for continuously preparing and gathering the superfine copper nano particles. Preferably, water and oleic acid are adopted as a solvent, so that the preparation method is enabled to be non-toxic and environmentally-friendly.
Description
Technical field
The present invention relates to a kind of preparation method of nano material, the method for ultra-fine copper nano particle is prepared in the liquid-liquid two-phase interface reaction of not dissolving each other of a kind of utilization specifically.
Background technology
Copper nano particles has unique catalysis characteristics, biological nature, optical characteristics and electrology characteristic due to dimensional effect, skin effect and quantum size effects, is widely used in the fields such as electronic manufacture, chemical analysis, biotechnology, anticorrosion and antifouling.The preparation method of conventional copper nano particles is a lot, as chemical reduction method, electrochemical reducing, gas-phase reaction method, evaporation or sputtering method, mechanical spheroidal graphite or comminuting method, laser ablation or high-energy radiation synthetic method etc.But still face many difficult problems in the Synthesis and applications process of current copper nano particles.The first is difficult to pattern and the size uniform of the nano particle ensureing to prepare.This point can be improved by strict control preparation condition such as temperature, the time etc. usually.It two is that the nanoparticle size for preparing is still larger.The copper nano particles size adopting existing method to prepare is many between 10-110nm, this makes the distinctive dimensional effect of nano material, skin effect and quantum size effects etc. are difficult to abundant realization, need to develop some controllabilitys good, simply, the novel processing step of low cost is to obtain the uniform copper nano particle [S.-H.Kwon of size at below 10nm, H.J.Choe, H.-C.Lee, C.-W.Chung, J.-J.Lee, ControlofSizeUniformityofCuNanoparticleArrayProducedbyPl asma-InducedDewetting, J.Nanosci.Nanotechnol.15 (2015) 2542 – 2546.doi:10.1166/jnn.2015.10237].It three is the reunions needing to prevent copper nano particles.Skin effect due to nano material makes tiny nano particle easily reunite, and causes the controllability of nanoparticle size, pattern and performance to be deteriorated; Reuniting also to make nano particle dispersedly cannot form stable dispersion liquid in a solvent.In order to prevent the reunion of nano particle, usually modify on the surface of nano particle, change its surface state, utilize charged group or long-chain organic matter (as CTAB, PVP etc.) to ensure that nano particle is in dispersity by electrostatic interaction or space steric effect.It four is the oxidations that must prevent copper nano particles.Under room temperature, copper nano particles just can oxidized generation cuprous oxide or cupric oxide in atmosphere, and make that its electric conductivity is deteriorated, the characteristic such as optics and catalysis changes.Common way is preparation under inert gas shielding or in vacuum, stores or use copper nano particles, but this can increase complexity and the cost of equipment and operation greatly.In the good inorganic material of the coated chemical stability of copper particle surface as silver, nickel, [the H.T.Hai such as carbon, H.Takamura, J.Koike, OxidationbehaviorofCu – Agcore – shellparticlesforsolarcellapplications, J.AlloysCompd.564 (2013) 71 – 77.doi:10.1016/j.jallcom.2013.02.048] [L.Ma, B.Yu, S.Wang, G.Su, H.Huang, H.Chen, etal., ControlledsynthesisandopticalpropertiesofCu/Ccore/shelln anoparticles, J.NanoparticleRes.16 (2014) 2545.doi:10.1007/s11051-014-2545-5], or coated CTAB, the organic matters such as PVP also can prevent or delay the oxidation [Y.Li of copper nano particles, D.Li, C.Li, H.Wang, D.Shen, L.Liu, etal., Annealing-inducedhighly-conductiveandstableCu – organiccompositenanoparticleswithhierarchicalstructures, J.AlloysCompd.636 (2015) 1 – 7.doi:10.1016/j.jallcom.2015.02.144].But coated way can increase cost equally, change the character of nano particle, and especially the organic coating thing of long-chain is difficult to remove in subsequent technique, thus cannot use in some applications.
Up to now, also do not have reliably, prepare the bibliographical information of particle diameter in the preparation method of the ultra-fine copper nano particle of below 10nm.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned problems of the prior art; there is provided a kind of and utilize the liquid that do not dissolve each other-liquid two-phase interface reaction; do not need protective gas or vacuum environment; technique is simple; low cost; practical, be applicable to the preparation method of quantity-produced ultra-fine copper nano particle.
The technical scheme that the present invention solves the problems of the technologies described above employing is: a kind of preparation method of ultra-fine copper nano particle, is characterized in that comprising the following steps:
1) reactant liquor is prepared: oil-soluble mantoquita be dissolved in non-polar solven the source liquid making cupric or oil-soluble mantoquita be first dissolved in the source liquid then making cupric in non-polar solven with polar solvent mixing and emulsifying; Water miscible reducing agent is dissolved in polar solvent and makes reducing solution;
2) reducing solution is added in the source liquid of cupric, form the two-phase system that do not dissolve each other be made up of the non-polar solution containing mantoquita and the polar solvent containing reducing agent; The two-phase system that will not dissolve each other stirs, vortex mixed or add ultrasonic and emulsification and form emulsion, emulsion droplet with form discontinuous stable liquid-liquid interface continuously; Or the two-phase system stratification that will not dissolve each other, make between the source liquid of cupric and reducing solution, to form continuous, large-area stable liquid-liquid interface; Or the two-phase system that do not dissolve each other is injected fine pipeline, form directed Laminar Flow, make streamwise between the source liquid of cupric and reducing solution form stable liquid-liquid interface;
3) reaction preparation: the above-mentioned two-phase system that do not dissolve each other containing liquid-liquid interface is remained on room temperature ~ 80
oat C temperature, there is redox reaction in above-mentioned liquid-liquid interface position, generate ultra-fine copper nano particle.
In step 1), described oil-soluble mantoquita, can be monovalence or cupric carboxylate, it be soluble in non-polar solven, and is slightly soluble in polar solvent, preferred copper oleate; The concentration of described oil-soluble mantoquita in the source liquid of cupric is preferably 0.001-0.2mol/L; Described reducing agent is hydrazine hydrate, inferior sodium phosphate, organo-metallic compound reducing agent, organic acid reduction agent, organic amine reducing agent or aldehydes reducing agent, or more the aqueous solution of reducing agent, its slightly soluble or be insoluble in non-polar solven, preferred ascorbic acid; The concentration of described reducing agent in reducing solution is preferably 0.005-1mol/L; The mol ratio of described mantoquita and reducing agent is less than 1.
In step 1), described non-polar solven is hydro carbons, halogenated hydrocarbon, benzene class, ethers, the alcohols of Long carbon chain, ketone, ester class, lipoidis and carbon disulfide, or their mixture, preferred oleic acid; Described polar solvent is the alcohols of water and short carbon chain, or their mixture, preferred water; Immiscible between described non-polar solven and polar solvent.
In step 1), the reproducibility power of described reducing solution can by regulating its pH value to control.
Further, in step 3), the temperature of described reaction preparation process is preferably 30 ~ 60
oc, described reaction preparation process controls by mass transport.
In step 3), the particle diameter≤10nm of described ultra-fine copper nano particle, it is strapped in liquid-liquid interface position by interfacial tension and does not reunite, can long-time preservation and not being oxidized in the two-phase system that do not dissolve each other after above-mentioned reaction preparation.
Compared with existing preparation method, preparation method of the present invention can simply utilize the redox reaction at the liquid that do not dissolve each other-liquid two-phase interface place to prepare the ultra-fine copper nano particle of size at below 10nm, impurity is few, pure, crystalline quality is good, the ultra-fine copper nanoparticle size obtained and pattern even, and without the need to adding not dissolving each other in two-phase system of obtaining after coating material and coated processing procedure are dispersed in reaction preparation with can making the ultra-fine copper nanoparticles stable obtained especially, and can place and not be oxidized for a long time under normal temperature, air conditions.This preparation method is simple, energy consumption is little, cost is low, equipment simply, easily controls, and has stronger practicality.The selectable range of polar solvent used and non-polar solven is wider, according to water and oleic acid as preferred solvent, can ensure nontoxic, environmental protection and have good bio-compatibility.If make liquid form continuous Laminar Flow in course of reaction, all right continuous production and collection ultra-fine copper nano particle, be applicable to continuous seepage.Adopt corresponding silver salt or other slaines to substitute mantoquita, ultra-fine silver nano particle or other ultra-fine metal nanoparticles can also be prepared by the method.
Detailed description of the invention
Embodiment 1: a kind of preparation method of ultra-fine copper nano particle, it comprises the following steps:
1) preparation of reactant liquor: under room temperature, copper oleate is dissolved in oleic acid, makes the oleic acid solutions that concentration is the copper oleate of 1.7mmol/L; The oleic acid solutions of 30ml copper oleate added in 30ml deionized water, the condition lower magnetic force of 1800rpm stirs 5 minutes, then uses the ultrasonic power of 20W ultrasonic 2 hours, leave standstill 24 hours, mixed liquor layering, upper strata is the oil phase of blue-tinted transparent, and lower floor is the opaque emulsion of micro-Huang; Remove upper oil phase with pipettor, remaining is stable oil-in-water emulsion, is namely the source liquid of cupric; Ascorbic acid is dissolved in deionized water, and making the Vitamin C aqueous acid that concentration is 1mol/L, is namely reducing solution;
2) not dissolve each other the formation of two-phase system and liquid-liquid interface: get above-mentioned oil-in-water emulsion 5ml, add Vitamin C aqueous acid 1ml, jiggle and make for 2-3 time it mix, obtain homogeneous latex emulsion, the two-phase system that do not dissolve each other namely for being formed by oleic acid solutions and the Vitamin C aqueous acid of copper oleate; Emulsion droplet is the oleic acid solutions of copper oleate, and continuous phase is Vitamin C aqueous acid, emulsion droplet with form discontinuous stable liquid-liquid interface continuously;
3) reaction preparation: the above-mentioned two-phase system that do not dissolve each other is placed in room temperature and leaves standstill 10 hours, obtain ultra-fine copper nano particle, what described ultra-fine copper nano particle obtained after being dispersed in reaction preparation does not dissolve each other in two-phase system.
Protective gas and vacuum is not added under room temperature; after the two-phase system that do not dissolve each other obtained after reaction preparation in embodiment 1 is placed 5 days; test through high-resolution-ration transmission electric-lens; the particle diameter of ultra-fine copper nano particle is 4-6nm; the pattern of ultra-fine copper nano particle is spherical substantially, and comparatively evenly, the spacing between two adjacent crystal planes is 2.09; corresponding to (111) face of Cu, be the measured fine copper nano particle of crystalline.Ultra-fine copper nano particle skin does not have obvious clad, but good dispersion, there is no agglomeration.Cu{111}, { 200}, { 220} and the { diffraction ring of 311} can be clear that in the SEAD style of ultra-fine copper nano particle, do not find the diffraction pattern of other materials, do not have oxide and other impurity of copper in gained ultra-fine copper nano particle, purity is higher.
Protective gas and vacuum is not added under room temperature; after the two-phase system that do not dissolve each other obtained after reaction preparation in embodiment 1 is placed 27 days; test through high-resolution-ration transmission electric-lens; particle diameter and the pattern of ultra-fine copper nano particle do not have significant change; also obviously do not reunite; spacing between two adjacent crystal planes is respectively 2.07 and 1.90, corresponding with (200) face to (111) face of Cu.Place in the SEAD style of ultra-fine copper nano particle after 27 days except Cu{111}, { 200}, { 220} and { diffraction ring of 311}, do not find the diffraction pattern of other materials, sample is not obviously oxidized.
Embodiment 2: a kind of preparation method of ultra-fine copper nano particle, it specifically comprises the following steps:
1) preparation of reactant liquor: under room temperature, copper oleate is dissolved in oleic acid, makes the oleic acid solutions that concentration is the copper oleate of 1.7mmol/L, is namely the source liquid of cupric; Ascorbic acid is dissolved in deionized water, and making the Vitamin C aqueous acid that concentration is 1mol/L, is namely reducing solution;
2) not dissolve each other the formation of two-phase system and liquid-liquid interface: under room temperature, in the sample bottle of 20ml, add 5ml Vitamin C aqueous acid; Then the oleic acid solutions 5ml slowly adding copper oleate along sample bottle sidewall is formed and not to dissolve each other two-phase system; The two-phase system that do not dissolve each other above is left standstill more than 5 minutes, lower leaf in the oleic acid solutions of aqueous ascorbic acid and copper oleate, and supernatant liquid is the oleic acid solutions of copper oleate, green transparent; Lower floor's liquid is aqueous ascorbic acid, water white transparency; The liquid-liquid interface that middle formation is stable, interface transparent;
3) reaction preparation: by taking advantage of the sample bottle bottle cap of the above-mentioned two-phase system that do not dissolve each other to tighten, be placed in 60
oin C water-bath, leave standstill 10 hours, supernatant liquid becomes blue-green transparency liquid, and lower floor's liquid becomes yellow transparent liquid, middle generate transparent and has the boundary layer of metallic luster, and boundary layer is formed by the ultra-fine copper nano-particles self assemble being dispersed in interface.
Embodiment 3: a kind of preparation method of ultra-fine copper nano particle, it comprises the following steps:
1) preparation of reactant liquor: under room temperature, copper oleate is dissolved in oleic acid, makes the oleic acid solutions that concentration is the copper oleate of 1.7mmol/L, is namely the source liquid of cupric; Ascorbic acid is dissolved in deionized water, and making the Vitamin C aqueous acid that concentration is 1mol/L, is namely reducing solution;
2) not dissolve each other the formation of two-phase system and liquid-liquid interface: under room temperature, get " Y " type microchannel, oil phase entrance and the aqueous phase inlet passageway width of this microchannel are 120 μm, and main channel width is 240 μm, and the height of passage is 10 μm everywhere.The oleic acid solutions of copper oleate is passed in the oil phase porch of microchannel; Vitamin C aqueous acid is passed in the aqueous phase porch of passage; Except atmospheric pressure, the pressure of 5kPa is separately added in the aqueous phase porch of " Y " type microchannel, except atmospheric pressure, the pressure of 12kPa is separately added in oil phase porch, the outlet of " Y " type microchannel and atmosphere, oleic acid solutions and the Vitamin C aqueous acid of copper oleate contact and form the two-phase system that do not dissolve each other in main channel, and form stable, parallel Laminar Flow.Through observation by light microscope, between the oleic acid solutions of copper oleate and Vitamin C aqueous acid, form stable liquid-liquid two-phase interface;
3) reaction preparation: under room temperature environment, keep above-mentioned Laminar Flow 10 hours, continuous production obtains ultra-fine copper nano particle; Ultra-fine copper nano particle arrives exit, " Y " type microchannel with flowing, is dispersed in the two-phase system that do not dissolve each other of oil phase and aqueous phase formation and is collected.
Embodiment 4: a kind of preparation method of ultra-fine copper nano particle, it comprises the following steps:
1) preparation of reactant liquor: under room temperature, copper oleate is dissolved in oleic acid, makes the oleic acid solutions that concentration is the copper oleate of 1.7mmol/L; The oleic acid solutions of 30ml copper oleate added in 30ml deionized water, the condition lower magnetic force of 1800rpm stirs 5 minutes, then uses the ultrasonic power of 20W ultrasonic 2 hours, leave standstill 24 hours, mixed liquor layering, upper strata is the oil phase of blue-tinted transparent, and lower floor is the opaque emulsion of micro-Huang; Remove upper oil phase with pipettor, remaining is stable oil-in-water emulsion, is namely the source liquid of cupric; Inferior sodium phosphate being dissolved in deionized water, making the aqueous solution that concentration is the inferior sodium phosphate of 1mol/L, is namely reducing solution;
2) not dissolve each other the formation of two-phase system and liquid-liquid interface: get above-mentioned oil-in-water emulsion 5ml, add the aqueous solution 1ml of inferior sodium phosphate, jiggle and make for 2-3 time it mix, obtain homogeneous latex emulsion, the two-phase system that do not dissolve each other namely for being formed by the oleic acid solutions of copper oleate and the aqueous solution of inferior sodium phosphate; Emulsion droplet is the oleic acid solutions of copper oleate, and continuous phase is the aqueous solution of inferior sodium phosphate, emulsion droplet with form discontinuous liquid-liquid interface continuously;
3) reaction preparation: the above-mentioned two-phase system that do not dissolve each other is placed in 30
oin C water-bath, leave standstill 10 hours, obtain ultra-fine copper nano particle, what described ultra-fine copper nano particle obtained after being dispersed in reaction preparation does not dissolve each other in two-phase system.
Embodiment 5: a kind of preparation method of ultra-fine copper nano particle, it comprises the following steps:
1) preparation of reactant liquor: under room temperature, copper oleate is dissolved in oleic acid, makes the oleic acid solutions that concentration is the copper oleate of 1.7mmol/L, is namely the source liquid of cupric; Trisodium citrate being dissolved in deionized water, making the aqueous solution that concentration is the trisodium citrate of 1mol/L, is namely reducing solution;
2) not dissolve each other the formation of two-phase system and liquid-liquid interface: under room temperature, in the sample bottle of 20ml, add the aqueous solution of 5ml trisodium citrate; Then the oleic acid solutions 5ml slowly adding copper oleate along sample bottle sidewall is formed and not to dissolve each other two-phase system; By not dissolving each other above, two-phase system leaves standstill more than 5 minutes, lower leaf in the aqueous solution of trisodium citrate and the oleic acid solutions of copper oleate, and supernatant liquid is the oleic acid solutions of copper oleate, green transparent; Lower floor's liquid is the aqueous solution of trisodium citrate, water white transparency; The liquid-liquid interface that middle formation is stable, interface transparent;
3) reaction preparation: the sample bottle bottle cap filling the above-mentioned two-phase system that do not dissolve each other is tightened, is placed in 80
oin C water-bath, leave standstill 8 hours, supernatant liquid becomes yellow green transparency liquid, and lower floor's liquid becomes pistac transparency liquid, and interface generates ultra-fine copper nano particle and is bound in interface.
Embodiment 6: a kind of preparation method of ultra-fine copper nano particle, it comprises the following steps:
1) preparation of reactant liquor: under room temperature, copper oleate is dissolved in n-hexane, makes the hexane solution that concentration is the copper oleate of 0.8mmol/L, is namely the source liquid of cupric; Ascorbic acid being dissolved in methyl alcohol, making the methanol solution that concentration is the ascorbic acid of 1mol/L, is namely reducing solution;
2) not dissolve each other the formation of two-phase system and liquid-liquid interface: under room temperature, in the sample bottle of 20ml, add the methanol solution of 5ml ascorbic acid; Then the hexane solution 5ml slowly adding copper oleate along sample bottle sidewall is formed and not to dissolve each other two-phase system; By not dissolving each other above, two-phase system leaves standstill more than 5 minutes, lower leaf on the methanol solution of ascorbic acid and the cyclohexane solution of copper oleate, and supernatant liquid is the cyclohexane solution of copper oleate, and pale bluish green is transparent; Lower floor's liquid is the methanol solution of ascorbic acid, water white transparency; Middle stabilizing solution-liquid the boundary layer forming width and be about 5mm, boundary layer pale yellow transparent;
3) reaction preparation: the sample bottle bottle cap filling the above-mentioned two-phase system that do not dissolve each other is tightened, room temperature leaves standstill 10 hours, supernatant liquid becomes oyster transparency liquid, lower floor's liquid is still colourless transparent liquid, intermediate layer is transparent and be faint yellow, and ultra-fine copper nano particle is dispersed in boundary layer.
Claims (7)
1. a preparation method for ultra-fine copper nano particle, is characterized in that comprising the following steps:
1) reactant liquor is prepared: oil-soluble mantoquita be dissolved in non-polar solven the source liquid making cupric or oil-soluble mantoquita be first dissolved in the source liquid then making cupric in non-polar solven with polar solvent mixing and emulsifying; Water miscible reducing agent is dissolved in polar solvent and makes reducing solution;
2) reducing solution is added in the source liquid of cupric, form the two-phase system that do not dissolve each other be made up of the non-polar solution containing mantoquita and the polar solvent containing reducing agent; The two-phase system that will not dissolve each other stirs, vortex mixed or add ultrasonic and emulsification and form emulsion, emulsion droplet with form discontinuous stable liquid-liquid interface continuously; Or the two-phase system stratification that will not dissolve each other, make between the source liquid of cupric and reducing solution, to form continuous, large-area stable liquid-liquid interface; Or the two-phase system that do not dissolve each other is injected fine pipeline, form directed Laminar Flow, make streamwise between the source liquid of cupric and reducing solution form stable liquid-liquid interface;
3) reaction preparation: the above-mentioned two-phase system that do not dissolve each other containing liquid-liquid interface is remained on room temperature ~ 80
oat C temperature, there is redox reaction in above-mentioned liquid-liquid interface position, generate ultra-fine copper nano particle.
2. the preparation method of ultra-fine copper nano particle according to claim 1, is characterized in that: in step 1), and described oil-soluble mantoquita is monovalence or cupric carboxylate; The concentration of described oil-soluble mantoquita in the source liquid of cupric is 0.001-0.2mol/L; Described reducing agent is hydrazine hydrate, inferior sodium phosphate, organo-metallic compound reducing agent, organic acid reduction agent, organic amine reducing agent or aldehydes reducing agent, or more the aqueous solution of reducing agent; The concentration of described reducing agent in reducing solution is preferably 0.005-1mol/L; The mol ratio of described mantoquita and reducing agent is less than 1.
3. the preparation method of ultra-fine copper nano particle according to claim 2, is characterized in that: the preferred copper oleate of described oil-soluble mantoquita; The preferred ascorbic acid of described reducing agent.
4. the preparation method of ultra-fine copper nano particle according to claim 1, it is characterized in that: in step 1), described non-polar solven is hydro carbons, halogenated hydrocarbon, benzene class, ethers, the alcohols of Long carbon chain, ketone, ester class, lipoidis and carbon disulfide, or their mixture; Described polar solvent is the alcohols of water and short carbon chain, or their mixture; Immiscible between described non-polar solven and polar solvent.
5. the preparation method of ultra-fine copper nano particle according to claim 4, is characterized in that: the preferred oleic acid of described non-polar solven; Described polar solvent preferred water.
6. the preparation method of ultra-fine copper nano particle according to claim 1, is characterized in that: in step 3), and the temperature of described reaction preparation process is preferably 30-60
oc, described reaction preparation process controls by mass transport.
7. the preparation method of ultra-fine copper nano particle according to claim 1, is characterized in that: in step 3), and the particle diameter≤10nm of described ultra-fine copper nano particle, it is strapped in liquid-liquid interface position by interfacial tension and does not reunite.
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| CN110744068B (en) * | 2019-10-21 | 2021-01-26 | 河南大学 | Oil-soluble nano copper and preparation method thereof |
| CN111672438A (en) * | 2020-06-17 | 2020-09-18 | 哈尔滨工业大学 | Method for preparing nano material based on microfluid device |
| CN112913857A (en) * | 2021-01-21 | 2021-06-08 | 周红岩 | Nano-copper antibacterial material, antibacterial coating, and preparation method and application thereof |
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