CN102294491B - Polliwog-shaped metal copper nanomaterial and preparation method thereof - Google Patents
Polliwog-shaped metal copper nanomaterial and preparation method thereof Download PDFInfo
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- CN102294491B CN102294491B CN 201010210041 CN201010210041A CN102294491B CN 102294491 B CN102294491 B CN 102294491B CN 201010210041 CN201010210041 CN 201010210041 CN 201010210041 A CN201010210041 A CN 201010210041A CN 102294491 B CN102294491 B CN 102294491B
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Abstract
The invention discloses a polliwog-shaped metal copper nanomaterial and a preparation method thereof, which fill the blank of the prior art at home and abroad and add a novel variety for a metal copper nanostructure material. The appearance of the metal copper nanostructure is polliwog-shaped; the structure is uniform and is mono-dispersed; the length of the polliwog-shaped material is about 4-5 micrometers; the head part of the polliwog-shaped material consists of hexagonal nanosheets of which the sizes are 600-800 nanometers; the body of the polliwog-shaped material consists of nanowires of which the diameters gradually decrease from the head part; the nanowires have high flexibility; and the tail part is crimped. The polliwog-shaped metal copper nanomaterial is prepared by adopting a microwave-assisted liquid phase reduction method in which a soluble copper salt, hexamethylene tetramine and ascorbic acid are taken as raw materials, water is taken as a solvent and a reaction mixed liquor undergoes a microwave radiation reduction reaction in a household microwave oven. The polliwog-shaped metal copper nanomaterial obtained with the method has a novel structure. The preparation method has the advantages of simple preparation process and equipment, readily available raw materials, low cost, mild reaction condition, no use of surfactant or organic solvent, low carbon, environmental friendliness, high repeatability and suitability for industrial production.
Description
Technical field
The present invention relates to belong to the nano material preparing technical field, specifically, relate to a kind of " tadpole " shape metallic copper nano material and preparation method thereof.
Background technology
Nanometer technology is the new and high technology of rising latter stage in 20th century, occupies consequence at material science.Copper nanoparticle is maroon, because size is little, specific area is large, the characteristics such as the Active sites number is many, resistance is little, quantum size effect, macro quanta tunnel effect, thereby show the new features that are different from conventional fine copper, have good catalysis, lubricated, conductivity, Application and Development widely.As synthesizing important chemical industrial product (such as acetylene polymerization) as catalyst; Be applied to gasoline engine lubricant oil or industrial lubricant as novel wearing and tearing repairing type lubricating additive, embodied good antifriction energy-saving, resistance to wear, the anti-extreme pressure energy; Be widely used in developing in electromagnetic shielding material and the electrically-conducting paint as conductive filler, alternative silver powder can make good and cheap conducting resinl of electric conductivity etc.Therefore, the development copper nanoparticle has important theory significance and practical value.
The preparation method of copper nanoparticle has a lot, mainly contains gas phase steam method, plasma method, mechanochemical reaction, gamma Rays-hydrothermal crystallization combination method etc., owing to all existing certain problem, promotes some difficulty.The unstrpped gas price that the gas phase steam method needs is high, equipment is complicated, cost is high; The capacity usage ratio of plasma method is low; Adopt the copper powder skewness of mechanochemical reaction preparation, particle diameter distributes wide, and easily introduces impurity; The standby powder of gamma-rays legal system is difficult to collect; And the most active with the research of Preparation of nanocrystalline copper powders by aqueous reduction, mainly be that equipment is simple, technological process is short, production cost is low, easy suitability for industrialized production.
Under nano materials research worker's unremitting effort, prepared the metallic copper nanostructured of different morphologies, such as nano particle, nanometer rods, nano wire, nanosphere, spindle and nanometer sheet etc.But, yet there are no the report of " tadpole " shape metallic copper nanostructured with regard to literature survey.
Summary of the invention
The object of the present invention is to provide a kind of " tadpole " shape metallic copper nano material and its preparation method, to fill up the blank of prior art, for the metallic copper nano structural material adds new varieties.
" tadpole " provided by the invention shape metallic copper nano material, it is characterized in that, described metallic copper nanostructured pattern is biological " tadpole " shape, structure homogeneous, the single dispersion, " tadpole " is about the 4-5 micron, and the head of " tadpole " is comprised of hexagonal nanometer sheet, is of a size of the 600-800 nanometer, the health of " tadpole " is comprised of nano wire, diameter reduces from the head gradually, and nano wire is better flexible, and afterbody is curling shape.
" tadpole " of the present invention shape metallic copper nano material adopts microwave auxiliary liquid phase reduction to prepare, namely, take soluble copper salt, hexamethylenetetramine and ascorbic acid as raw material, water is solvent, and reaction mixture is formed through microwave irradiation reduction reaction process in the family expenses micro-wave oven.Its concrete technology flow process is as follows:
(1) take by weighing in the high pin flask of anhydrous cupric sulfate and ascorbic acid to 100 milliliter, add 30 ml deionized water, stirring and dissolving gets solution A;
(2) take by weighing in the beaker of hexamethylenetetramine to 50 milliliter, add 30 ml deionized water, stirring and dissolving gets solution B;
(3) solution B is joined in the solution A, cover with polyethylene film, reaction mixture continues to stir 10～20 minutes;
(4) reaction mixture is placed micro-wave oven, low fire screen heating 6～30 minutes;
(5) naturally cool to room temperature, filtering precipitate is used respectively deionized water and absolute ethanol washing 3～5 times;
(6) sediment is placed vacuum drying chamber heated 6～12 hours, temperature is 40～60 ℃, collects product and namely obtains described " tadpole " shape metallic copper nano material.
In the technique scheme, described anhydrous cupric sulfate and ascorbic acid mol ratio are 1: 2.
The amount of substance of described anhydrous cupric sulfate and hexamethylenetetramine is 1: 24～36.
Described micro-wave oven is the commercialization household microwave oven, microwave output power 800W.
" tadpole " shape metallic copper nano material that the present invention obtains is a kind of metallic copper nano material with novel structure, can lead at electricity, be developed and applied in the fields such as catalysis, lubricated, sterilization.Described preparation technology's equipment is simple, and environment temperature is low, and is easy and simple to handle, good reproducibility; Do not adopt organic solvent and surfactant, the environmental friendliness cleaning; With short production cycle, productive rate is high, raw material is easy to get, and is with low cost, suitability for industrialized production.
Compare with existing metallic copper nanostructured and technology of preparing thereof, beneficial effect of the present invention is embodied in:
(1) the present invention has adopted without template Green Chemistry method and has prepared novel metallic copper nanostructured, has increased the Nanometer Copper family member.
The inventive method adopts Microwave Radiation in Manufacturing, and is simple to operate, is swift in response, easy to operate, low-carbon high-efficiency.This method requires easily realization to temperature, raw material etc., and cost is low, suitability for industrialized production.
Description of drawings
Fig. 1 is X-ray diffraction analysis (XRD) figure of the present invention " tadpole " shape metallic copper nano material;
Fig. 2 is field emission scanning electron microscope (SEM) photo of the present invention " tadpole " shape metallic copper nano material;
Fig. 3 is transmission electron microscope (TEM) photo of the present invention " tadpole " shape metallic copper nano material;
Fig. 4 is field emission scanning electron microscope (FESEM) photo of single " tadpole " of the present invention " tadpole " shape metallic copper nano material.
The specific embodiment
Below technical scheme of the present invention is done the description of further detailed complete by specific embodiment.Following embodiment further specifies of the present invention, and does not limit the scope of the invention.
Embodiment 1
" tadpole " of the present invention shape metallic copper nano material adopts microwave auxiliary liquid phase reduction to prepare, namely, take soluble copper salt, hexamethylenetetramine and ascorbic acid as raw material, water is solvent, and reaction mixture is formed through microwave irradiation reduction reaction process in the family expenses micro-wave oven.Its concrete technology flow process is as follows:
(1) take by weighing in the high pin flask of 0.1596 gram anhydrous cupric sulfate and 0.348 gram ascorbic acid to 100 milliliter, add 30 ml deionized water, stirring and dissolving gets solution A;
(2) take by weighing in the beaker of 4.48 gram hexamethylenetetramines to 50 milliliter, add 30 ml deionized water, stirring and dissolving gets solution B;
(3) solution B is joined in the solution A, cover with polyethylene film, reaction mixture continues to stir 10～20 minutes;
(4) reaction mixture is placed micro-wave oven, low fire screen heating 15 minutes;
(5) naturally cool to room temperature, filtering precipitate is used respectively deionized water and absolute ethanol washing 3～5 times;
(6) sediment is placed vacuum drying chamber heating 6 hours, temperature is 60 ℃, collects product and namely obtains described " tadpole " shape metallic copper nano material.
Referring to accompanying drawing 1, X-ray diffraction (XRD) figure of " tadpole " shape metallic copper nano material that makes by embodiment 1 described method, the spectral line peak position is corresponding one by one with the diffraction maximum of the metallic copper of JCPDS card (04-836) among the figure, is indicated as the elemental copper of face-centered cubic phase structure.
Referring to accompanying drawing 2, field emission scanning electron microscope (FESEM) photo of " tadpole " shape metallic copper nano material that makes by embodiment 1 described method, the output of visible metallic copper nanostructured is high, and pattern is single.
Referring to accompanying drawing 3, transmission electron microscope (TEM) photo of " tadpole " shape metallic copper nano material that makes by embodiment 1 described method, as seen metallic copper nanostructured pattern is biological " tadpole " shape, good dispersion, and " tadpole " is about the 4-5 micron, the head of " tadpole " is comprised of hexagonal nanometer sheet, be of a size of the 600-800 nanometer, the health of " tadpole " is comprised of nano wire, and diameter reduces from the head gradually, nano wire is better flexible, and afterbody is curling shape.
Referring to accompanying drawing 4, field emission scanning electron microscope (FESEM) photo of single " tadpole " of " tadpole " shape metallic copper nano material that makes by embodiment 1 described method, as seen the health of " tadpole " is that the middle part growth of nanometer sheet from the head forms, by slightly gradually thin, afterbody occurs curling.
" tadpole " of the present invention shape metallic copper nano material adopts microwave auxiliary liquid phase reduction to prepare, namely, take soluble copper salt, hexamethylenetetramine and ascorbic acid as raw material, water is solvent, and reaction mixture is formed through microwave irradiation reduction reaction process in the family expenses micro-wave oven.Its concrete technology flow process is as follows:
(1) take by weighing in the high pin flask of 0.1594 gram anhydrous cupric sulfate and 0.346 gram ascorbic acid to 100 milliliter, add 30 ml deionized water, stirring and dissolving gets solution A;
(2) take by weighing in the beaker of 3.36 gram hexamethylenetetramines to 50 milliliter, add 30 ml deionized water, stirring and dissolving gets solution B;
(3) solution B is joined in the solution A, cover with polyethylene film, reaction mixture continues to stir 10～20 minutes;
(4) reaction mixture is placed micro-wave oven, low fire screen heating 6 minutes;
(5) naturally cool to room temperature, filtering precipitate is used respectively deionized water and absolute ethanol washing 3～5 times;
(6) sediment is placed vacuum drying chamber heating 12 hours, temperature is 60 ℃, collects product and namely obtains described " tadpole " shape metallic copper nano material.
Observe through FESEM, by embodiment 2 described methods make for being biology " tadpole " shape metallic copper nano material.
Embodiment 3
" tadpole " of the present invention shape metallic copper nano material adopts microwave auxiliary liquid phase reduction to prepare, namely, take soluble copper salt, hexamethylenetetramine and ascorbic acid as raw material, water is solvent, and reaction mixture is formed through microwave irradiation reduction reaction process in the family expenses micro-wave oven.Its concrete technology flow process is as follows:
(1) take by weighing in the high pin flask of 0.1597 gram anhydrous cupric sulfate and 0.349 gram ascorbic acid to 100 milliliter, add 30 ml deionized water, stirring and dissolving gets solution A;
(2) take by weighing in the beaker of 5.04 gram hexamethylenetetramines to 50 milliliter, add 30 ml deionized water, stirring and dissolving gets solution B;
(3) solution B is joined in the solution A, cover with polyethylene film, reaction mixture continues to stir 10～20 minutes;
(4) reaction mixture is placed micro-wave oven, low fire screen heating 20 minutes;
(5) naturally cool to room temperature, filtering precipitate is used respectively deionized water and absolute ethanol washing 3～5 times;
(6) sediment is placed vacuum drying chamber heating 10 hours, temperature is 60 ℃, collects product and namely obtains described " tadpole " shape metallic copper nano material.
Observe through FESEM, by embodiment 2 described methods make for being biology " tadpole " shape metallic copper nano material.
Claims (5)
1. " tadpole " shape metallic copper nano material, it is characterized in that, described metallic copper nanostructured pattern is biological " tadpole " shape, structure homogeneous, the single dispersion, " tadpole " is about the 4-5 micron, and the head of " tadpole " is comprised of hexagonal nanometer sheet, is of a size of the 600-800 nanometer, the health of " tadpole " is comprised of nano wire, diameter reduces from the head gradually, and nano wire is better flexible, and afterbody is curling shape.
2. " tadpole " claimed in claim 1 shape metallic copper preparations of nanomaterials method is characterized in that, described method comprises following concrete steps:
(1) take by weighing in the high pin flask of anhydrous cupric sulfate and ascorbic acid to 100 milliliter, add 30 ml deionized water, stirring and dissolving gets solution A; Take by weighing in the beaker of hexamethylenetetramine to 50 milliliter, add 30 ml deionized water, stirring and dissolving gets solution B;
(2) solution B is joined in the solution A, cover with polyethylene film, reaction mixture continues to stir 10～20 minutes;
(3) reaction mixture is placed micro-wave oven, low fire screen heating 6～30 minutes;
(4) naturally cool to room temperature, filtering precipitate is used respectively deionized water and absolute ethanol washing 3～5 times;
(5) sediment is placed vacuum drying chamber heated 6～12 hours, temperature is 40～60 ℃, collects product and namely obtains described " tadpole " shape metallic copper nano material.
3. " tadpole " according to claim 2 shape metallic copper preparations of nanomaterials method, it is characterized in that: anhydrous cupric sulfate and ascorbic acid mol ratio are 1: 2 described in the step (1).
4. " tadpole " according to claim 2 shape metallic copper preparations of nanomaterials method, it is characterized in that: the amount of substance of anhydrous cupric sulfate and hexamethylenetetramine is 1: 32 described in the step (1).
5. " tadpole " according to claim 2 shape metallic copper preparations of nanomaterials method, it is characterized in that: micro-wave oven is the commercialization household microwave oven described in the step (3), and microwave output power 800W was low fire screen heating 15 minutes.
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| CN104148669B (en) * | 2014-08-29 | 2016-11-02 | 厦门大学 | A kind of preparation method of bimetal nano line |
| CN112296346B (en) * | 2019-07-25 | 2023-05-19 | 上海沪正实业有限公司 | Nanometer copper powder and application thereof in preparation of copper-containing fiber antibacterial deodorizing sock |
| CN110465653B (en) * | 2019-09-19 | 2021-11-05 | 安徽工业大学 | Silver wire and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007120193A2 (en) * | 2005-11-01 | 2007-10-25 | University Of South Carolina | Bionanomaterials and their synthesis |
| CN101433966A (en) * | 2008-12-17 | 2009-05-20 | 江西农业大学 | Method for preparing tadpole-shaped gold nanoparticle using ultrasonic promoted aqueous phase soft moulding plate method |
| WO2009085017A1 (en) * | 2008-01-03 | 2009-07-09 | Agency For Science, Technology And Research | Mesoporous nanostructures |
| CN101618461A (en) * | 2009-08-12 | 2010-01-06 | 吉林大学 | Preparation method of calabash-shaped, dumbbell-shaped or bar-shaped gold nano-particles |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007120193A2 (en) * | 2005-11-01 | 2007-10-25 | University Of South Carolina | Bionanomaterials and their synthesis |
| WO2009085017A1 (en) * | 2008-01-03 | 2009-07-09 | Agency For Science, Technology And Research | Mesoporous nanostructures |
| CN101433966A (en) * | 2008-12-17 | 2009-05-20 | 江西农业大学 | Method for preparing tadpole-shaped gold nanoparticle using ultrasonic promoted aqueous phase soft moulding plate method |
| CN101618461A (en) * | 2009-08-12 | 2010-01-06 | 吉林大学 | Preparation method of calabash-shaped, dumbbell-shaped or bar-shaped gold nano-particles |
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