CN107498068A - A kind of preparation method of flower-like nanometer copper - Google Patents
A kind of preparation method of flower-like nanometer copper Download PDFInfo
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- CN107498068A CN107498068A CN201710868958.6A CN201710868958A CN107498068A CN 107498068 A CN107498068 A CN 107498068A CN 201710868958 A CN201710868958 A CN 201710868958A CN 107498068 A CN107498068 A CN 107498068A
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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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- 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
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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
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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Abstract
A kind of preparation method of flower-like nanometer copper, belong to it is micro-/receive technical field of material.Concretely comprise the following steps：Prepare soluble cupric salt solution and ortho phosphorous acid sodium solution, prevent Nanometer Copper from reuniting and aoxidizing in preparation process with surfactant-dispersed agent and protective agent, then preheated under 30 DEG C of 150 DEG C of water bath conditions, the two is well mixed after reaching predetermined temperature, reaction a period of time solution presentation claret is to have flower-like nanometer copper particles generation, and washing centrifugation dries 46 hours as finished products after 50 DEG C in vacuum drying chamber.The present invention is to react gentle sodium hypophosphite as reducing agent, avoid the potential safety hazard for using strong reductant to bring, and this technique is simple and reproducible, the flower-like nanometer copper product of preparation has structure novel, and pattern is uniform in size, good dispersion, purity is high, and there is certain oxidation resistance, it can be applied to mass produce, be adapted to do catalyst, conductive filler, anti-corrosive antibacterial material and heat conduction abrasion-resistant material etc..
Description
Technical field
The present invention relates to a kind of preparation method of flower-like nanometer copper, belong to it is micro-/receive technical field of material.
Background technology
Lot of documents research shows that the pattern and size of material are very big to the performance impact of material, especially when material
When yardstick drops to nanometer, the characteristic such as optics, calorifics, magnetics and its biology of material compared with the macroscopic material of routine,
Significant change occurs.The application of nanometer technology so that the development of functional material becomes more rapid, and has driven many height
The fast development of new technical field, this just makes nano material have broader practice prospect.
Nanometer Copper has good electric conductivity, catalytic performance and optical property etc., nanometer as a kind of copper nano material
Its particle of copper powder is minimum and soft texture, has good wear-resistant wearability, and a kind of good lube oil additive.Nanometer
Copper powder is used to manufacture electrocondution slurry, can increase substantially the electric conductivity of material, and price is less than other noble metals（As silver and
Palladium etc.）, there is high application value in Electronic Packaging field, microelectronic and field of powder metallurgy.Copper nanoparticle chi
Very little small, specific surface area is big, surface atom ligancy wretched insufficiency, and the defects of a large amount of be present, thus with catalytic activity height, choosing
Selecting property is good and the features such as high catalytic efficiency, copper nanoparticle can improve reaction efficiency, controlling reaction temperature, optimization as catalyst
Reaction path, or even make what can not be carried out originally to be reacted to possibility, make it increasingly deep in the research and application of catalytic field
And expansion.
At present, had been developed that various methods prepare the copper nanostructured of novel in shape, had nanosphere, nanometer rods, receive
Mitron, nano wire, nanometer sheet, how empty cube and the multilevel hierarchy being self-assembly of with copper nano particles, and it is three-dimensional flower-shaped
Structural nano copper also rarely has report.
The content of the invention
It is an object of the invention to propose a kind of preparation method of flower-like nanometer copper.The preparation method uses water-bath or oil
Heating condition is bathed, reactant is stirred mixing, flower-like nanometer copper is restored with liquid phase reduction, realizes that Nanometer Copper can control
Standby process.The preparation method technique is simple, and size is controllable, purity is high and can be applied to mass produce.
The technical solution adopted by the present invention is：A kind of preparation method of flower-like nanometer copper, comprises the following steps：
Step 1, cupric salt is dissolved in the cupric salt precursor solution for being made into that concentration is 0.05-10mol/L in solvent, then
Surfactant is added in cupric salt precursor solution, dosage of surfactant is the 5-20% of cupric salt quality used,
It is standby that obtained mixed liquor is heated to 30-150 DEG C of temperature；
Step 2, reducing agent sodium hypophosphite is dissolved in solvent, is configured to 0.05-10mol/L reductant solution, and adjust
Whole pH value, make it that it is standby to be preheating to 30-150 DEG C of temperature in 2-5 sour environments；
Step 3, the rotating speed by cupric salt precursor solution and reductant solution in mixing in rotating speed for 200-1000r/min
Under stir, the mol ratio of cupric salt and reducing agent is 1:1-1:10, and under the conditions of 30-150 DEG C of water-bath or oil bath
10-240min is incubated, solution is changed into claret product, the constant maintenance reaction 10-30min of keeping temperature from blueness；
Step 4, the product are used respectively after deionized water washing 3-5 times, absolute ethyl alcohol wash 3-5 times by centrifuging
Vacuum drying chamber obtains flower-like nanometer copper finished product in 50 DEG C of dry 4-6h.
The cupric salt selects copper nitrate, copper sulphate or copper acetate.
The solvent is from deionized water, ethanol, ethylene glycol, benzene, toluene.
The surfactant is from polyvinylpyrrolidone, citric acid, neopelex, cetyl front three
Base ammonium bromide, gelatin or oleic acid.
The hybrid mode of the cupric salt solution and reductant solution is to be added dropwise or directly mix.
The design of patent of the present invention is as follows：The present invention is using relatively strong and safety and stability the ortho phosphorous acid sodium reduction of reducing property
Agent, and realize Cu in the case where cupric salt precursor solution and sodium hypophosphite reductant solution concentration are higher2+Also
Former process, cause in the case of reducing agent abundance in Cu2+Being reduced into copper simple substance has a large amount of Nanometer Copper nucleus to generate initial stage, to the greatest extent
Pipe in this way, but too high cupric salt concentration, make Cu2+Concentration is maintained at hypersaturated state, so that copper nucleus continues a large amount of lifes
Into, therefore its growth course is suppressed, simultaneously because Nanometer Copper nucleus diamter is minimum, surface energy is high, extremely unstable, Zhi Nengtong
Cross and fit together reduction surface energy, stablize three-dimensional flower-shaped structure so as to be formed.Liquid phase method is current laboratory and industrial system
Standby nano copper particle often dissolves with one of main method, in particular to by suitable soluble metallic salt, makes by all means
Bivalent cupric ion reduces the particle to be formed with definite shape and size in the solution, then obtains ultra-fine copper particles by post processing
Method, have accurately control chemical composition, quantitatively adulterate with the good compound particle of processability, the nanometer of preparation
Grain surface-active is high, and purity height is easily controlled the shape and granularity of particle, and equipment is simple, and technological process is short and is easy to industrialize
The features such as production.
The beneficial effects of the invention are as follows：Flower-like nanometer copper is prepared using the chemical reduction method of simplicity, with prior art phase
Than having the advantage that：
（1）Technological process is simple and easy to do, and reaction condition is gentle, and the reaction time is short, can synthesize at a lower temperature with complexity
The flower-like nanometer copper of pattern.
（2）Equipment is simple, it is not necessary to the large-scale instrument and equipment of complex precise, reduces investment of production cost and operating cost
With.
（3）Excellent product performance, it can be seen that the Nanometer Copper pattern prepared is three-dimensional flower-shaped structure from SEM pictures, grain
Footpath is uniform, from TEM it can be seen that flower-like nanometer copper is the little particle for having many 5-10nm assembles, therefore three-dimensional flower-shaped structure
With bigger surface-active and surface roughness.From XRD as can be seen that only the diffraction maximum of copper, no cupric oxide spread out
Peak appearance is penetrated, the flower-like nanometer copper purity high-crystallinity that surface is made is good, and just has certain oxidation resistance.
Brief description of the drawings
Fig. 1 is the XRD spectra of flower-like nanometer copper.
Fig. 2 is the SEM scanning electron microscope (SEM) photographs of flower-like nanometer copper.
Fig. 3 is the TEM transmission electron microscope pictures of flower-like nanometer copper.
Embodiment
With reference to embodiment, the present invention is described in detail, and embodiment is only the preferred embodiment of the present invention, no
It is limitation of the invention.
Embodiment 1
（1）Now by CuSO4·5H2It is 0.1mol/L cupric salt solution that O, which is made into molar concentration, then is added in cupric salt
Surfactant, dosage of surfactant are the 5% of cupric salt quality used, and by obtained mixed liquor be heated to 60 DEG C it is standby
With.
（2）Reducing agent sodium hypophosphite is dissolved in deionized water, is configured to 0.1mol/L solution, and adjusts PH
Value, make it that it is standby to be preheating to certain temperature in 2-4 sour environments.
（3）The cupric salt precursor solution and reductant solution of same volume are taken respectively, are in rotating speed in mixing
Stirred under 600r/min rotating speed, 120min or so, solution is changed into claret from blueness, illustrates there is Nanometer Copper life in solution
Into, and it is incubated maintenance reaction 50min at 60 DEG C；
（4）By above step products therefrom respectively after deionized water washing 3-5 times, absolute ethyl alcohol wash 3-5 times by centrifugation
Separation, with vacuum drying chamber in 50 DEG C of dry 4-6h, you can obtain flower-like nanometer copper finished product.
Embodiment 2
（1）Now by CuSO4·5H2It is 0.2mol/L cupric salt solution that O, which is made into molar concentration, then table is added in cupric salt
Face activating agent, dosage of surfactant is the 10% of cupric salt quality used, and obtained mixed liquor is heated into certain temperature
60 DEG C standby.
（2）Reducing agent sodium hypophosphite is dissolved in deionized water, is configured to 0.2mol/L solution, and adjusts PH
Value, make it that it is standby to be preheating to certain temperature in 2-4 sour environments.
（5）Cupric salt precursor solution and reductant solution volume ratio are 1:2, in rotating speed it is 600r/ in mixing
Stirred under min rotating speed, and 60min or so is incubated under the conditions of 60 DEG C of water-baths or oil bath, solution is changed into wine from blueness
Red, illustrate there is Nanometer Copper generation in solution, and maintenance reaction 50min is incubated at 60 DEG C；
（3）By the product obtained by above step respectively through deionized water wash 3-5 time, absolute ethyl alcohol washing 3-5 times after by from
The heart separates, with vacuum drying chamber in 50 DEG C of dry 4-6h, you can obtain flower-like nanometer copper.
Embodiment 3
（1）Now by CuSO4·5H2It is 0.3mol/L cupric salt solution that O, which is made into molar concentration, then table is added in cupric salt
Face activating agent, dosage of surfactant is the 15% of cupric salt quality used, and obtained mixed liquor is heated into certain temperature
80 DEG C standby.
（2）Reducing agent sodium hypophosphite is dissolved in deionized water, is configured to 0.3mol/L solution, and adjusts PH
Value, make it that it is standby to be preheating to certain temperature in 2-4 sour environments.
（6）The cupric salt precursor solution and reductant solution of same volume are taken respectively, are in rotating speed in mixing
Stirred under 500r/min rotating speed, and keep 80 DEG C of certain temperature constant under the conditions of water-bath or oil bath, 20min is left
The right side, solution are changed into claret from blueness, illustrate there is Nanometer Copper generation in solution, and are incubated maintenance reaction 50min at 60 DEG C；
（3）By above step products therefrom respectively after deionized water washing 3-5 times, absolute ethyl alcohol wash 3-5 times by centrifugation
Separation, with vacuum drying chamber in 50 DEG C of dry 4-6h, you can obtain flower-like nanometer copper.
Embodiment 4
（1）Now by CuSO4·5H2It is 0.4mol/L cupric salt solution that O, which is made into molar concentration, then table is added in cupric salt
Face activating agent, dosage of surfactant is the 20% of cupric salt quality used, and obtained mixed liquor is heated into certain temperature
90 DEG C standby.
（2）Reducing agent sodium hypophosphite is dissolved in deionized water, is configured to 0.4mol/L solution, and adjusts PH
Value, make it that it is standby to be preheating to certain temperature in 2-4 sour environments.
（7）The cupric salt precursor solution and reductant solution of same volume are taken respectively, are in rotating speed in mixing
Stirred under 400r/min rotating speed, and keep 90 DEG C of certain temperature constant under the conditions of water-bath or oil bath, 10min is left
The right side, solution are changed into claret from blueness, illustrate there is Nanometer Copper generation in solution, and are incubated maintenance reaction 50min at 60 DEG C；
（3）By above step products therefrom respectively after deionized water washing 3-5 times, absolute ethyl alcohol wash 3-5 times by centrifugation
Separation, with vacuum drying chamber in 50 DEG C of dry 4-6h, you can obtain flower-like nanometer copper.
Claims (5)
1. a kind of preparation method of flower-like nanometer copper, it is characterized in that：Comprise the following steps：
Step 1, cupric salt is dissolved in the cupric salt precursor solution for being made into that concentration is 0.05-10mol/L in solvent, then
Surfactant is added in cupric salt precursor solution, dosage of surfactant is the 5-20% of cupric salt quality used,
It is standby that obtained mixed liquor is heated to 30-150 DEG C of temperature；
Step 2, reducing agent sodium hypophosphite is dissolved in solvent, is configured to 0.05-10mol/L reductant solution, and adjust
Whole pH value, make it that it is standby to be preheating to 30-150 DEG C of temperature in 2-5 sour environments；
Step 3, the rotating speed by cupric salt precursor solution and reductant solution in mixing in rotating speed for 200-1000r/min
Under stir, the mol ratio of cupric salt and reducing agent is 1:1-1:10, and under the conditions of 30-150 DEG C of water-bath or oil bath
10-240min is incubated, generates nanometer copper product in the solution, solution is changed into claret from blueness, is incubated 10-30min；
Step 4, the product are used respectively after deionized water washing 3-5 times, absolute ethyl alcohol wash 3-5 times by centrifuging
Vacuum drying chamber obtains flower-like nanometer copper finished product in 50 DEG C of dry 4-6h.
2. a kind of preparation method of flower-like nanometer copper according to claim 1, it is characterized in that：The cupric salt selects nitre
Sour copper, copper sulphate or copper acetate.
3. a kind of preparation method of flower-like nanometer copper according to claim 1, it is characterized in that：The solvent selects deionization
Water, ethanol, ethylene glycol, benzene, toluene.
4. a kind of preparation method of flower-like nanometer copper according to claim 1, it is characterized in that：The surfactant is selected
Polyvinylpyrrolidone, citric acid, neopelex, cetyl trimethylammonium bromide, gelatin or oleic acid.
5. a kind of preparation method of flower-like nanometer copper according to claim 1, it is characterized in that：The cupric salt solution and
The hybrid mode of reductant solution is to be added dropwise or directly mix.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108277458A (en) * | 2018-04-25 | 2018-07-13 | 河南科技大学 | A method of preparing free state flower-shape copper particle without template |
| CN109822108A (en) * | 2018-11-27 | 2019-05-31 | 西安航天化学动力有限公司 | A kind of nano copper particle preparation method of the surface with bayonet fittings |
| CN110026550A (en) * | 2018-11-07 | 2019-07-19 | 扬州工业职业技术学院 | A kind of nano zero-valence copper and preparation method and application |
| CN113000855A (en) * | 2021-03-23 | 2021-06-22 | 中国科学技术大学先进技术研究院 | Preparation method of micro-nano copper powder |
| CN113084186A (en) * | 2021-03-30 | 2021-07-09 | 武汉大学 | Flower-shaped copper particle and preparation method thereof |
| CN114535863A (en) * | 2022-03-25 | 2022-05-27 | 重庆平创半导体研究院有限责任公司 | Self-sintered nano-copper soldering paste, preparation method and use method thereof |
| CN114892300A (en) * | 2022-06-02 | 2022-08-12 | 浙江理工大学 | Preparation method of antibacterial antiviral thermal fiber |
| CN115028187A (en) * | 2022-08-02 | 2022-09-09 | 沈阳工业大学 | Chemical preparation method of copper oxide nanoparticles |
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| CN102198513A (en) * | 2011-05-27 | 2011-09-28 | 中南大学 | Method for preparing nano copper particle |
| CN102601381A (en) * | 2012-03-11 | 2012-07-25 | 郭雨 | Copper nano powder and preparation method of copper nano powder |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108277458B (en) * | 2018-04-25 | 2020-01-07 | 河南科技大学 | Method for preparing free-form flower-shaped copper particles without template |
| CN108277458A (en) * | 2018-04-25 | 2018-07-13 | 河南科技大学 | A method of preparing free state flower-shape copper particle without template |
| CN110026550A (en) * | 2018-11-07 | 2019-07-19 | 扬州工业职业技术学院 | A kind of nano zero-valence copper and preparation method and application |
| CN109822108A (en) * | 2018-11-27 | 2019-05-31 | 西安航天化学动力有限公司 | A kind of nano copper particle preparation method of the surface with bayonet fittings |
| CN113000855B (en) * | 2021-03-23 | 2024-04-19 | 中国科学技术大学先进技术研究院 | Preparation method of micro-nano copper powder |
| CN113000855A (en) * | 2021-03-23 | 2021-06-22 | 中国科学技术大学先进技术研究院 | Preparation method of micro-nano copper powder |
| CN113084186A (en) * | 2021-03-30 | 2021-07-09 | 武汉大学 | Flower-shaped copper particle and preparation method thereof |
| CN114535863A (en) * | 2022-03-25 | 2022-05-27 | 重庆平创半导体研究院有限责任公司 | Self-sintered nano-copper soldering paste, preparation method and use method thereof |
| CN114535863B (en) * | 2022-03-25 | 2024-01-16 | 重庆平创半导体研究院有限责任公司 | Self-sintered nano copper soldering paste, preparation method and use method thereof |
| CN114892300A (en) * | 2022-06-02 | 2022-08-12 | 浙江理工大学 | Preparation method of antibacterial antiviral thermal fiber |
| CN114892300B (en) * | 2022-06-02 | 2024-05-28 | 浙江理工大学 | Preparation method of antibacterial antiviral thermal fiber |
| CN115028187A (en) * | 2022-08-02 | 2022-09-09 | 沈阳工业大学 | Chemical preparation method of copper oxide nanoparticles |
| CN115028187B (en) * | 2022-08-02 | 2024-04-19 | 沈阳工业大学 | Chemical preparation method of copper oxide nano particles |
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