CN107344729A - A kind of preparation method of CuO nanometer rods - Google Patents
A kind of preparation method of CuO nanometer rods Download PDFInfo
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- CN107344729A CN107344729A CN201710633070.4A CN201710633070A CN107344729A CN 107344729 A CN107344729 A CN 107344729A CN 201710633070 A CN201710633070 A CN 201710633070A CN 107344729 A CN107344729 A CN 107344729A
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- C—CHEMISTRY; METALLURGY
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- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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Abstract
The present invention provides a kind of preparation method of CuO nanometer rods, belongs to nano inorganic metal oxide preparing technical field.The preparation method of the CuO nanometer rods, the organic solvent of alkali is instilled in the organic solvent of mantoquita, obtain the solidliquid mixture containing blue precipitate, pure water is added in foregoing solidliquid mixture, obtain the solidliquid mixture containing CuO precipitations, centrifuge washing and after drying obtains CuO nanometer rods.The preparation method for the CuO nanometer rods that the application provides, using liquid phase synthesizing method, cost is low, controllability is good, operability is simple and convenient, by the regulation and control to mantoquita species, reactant concentration, reaction temperature, purity height, the CuO nanometer rods of size uniform are prepared, the CuO nanorod diameters prepared are less than 15nm.
Description
Technical field
The present invention relates to the preparing technical field of nano inorganic metal oxide, more particularly to a kind of system of CuO nanometer rods
Preparation Method.
Background technology
Literature research shows：The performance of material and the size of its microscopic structural units are closely related.Due to CuO ratio surface
Product sharply increases with the reduction of its crystallite dimension so that and nanometer CuO generates the special effects not available for its cake mass,
Such as skin effect, small-size effect and macro quanta tunnel effect.So nanometer CuO in high-temperature superconductor, electronic device, urge
Agent, sensor, antibacterial and deodorization etc. have the incomparable properties of general block CuO.
, generally will in involved preparation technology in order to obtain the CuO of special appearance and nano-scale in existing report
Surfactant and template are added, but the surfactant and template that add have the shortcomings that being difficult to thoroughly remove, shadow
Product purity is rung, then reduces the performance of nanometer CuO.So exploitation a kind of " green ", without any surfactant
It is particularly important with the preparation method of the nanometer CuO of template.
The content of the invention
The problem to be solved in the present invention is the preparation method of existing nanometer CuO, adds surfactant and template, shadow
Ring the performance of nanometer CuO.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of preparation side of CuO nanometer rods is provided
Method.The preparation method of the CuO nanometer rods, comprises the following steps：
(1) organic solution of cupric salt is prepared：The organic solution of cupric salt is prepared with organic solvent, makes Cu2+Rub
Your concentration is 0.001~0.1mol/L, and cupric salt solution is stirred and heated into 60~78 DEG C, is denoted as solution A；
Described cupric salt is Cu (NO3)2、Cu(CH3COO)2、CuSO4、CuCl2In one or more of mixtures；
(2) organic solution of alkaline is matched somebody with somebody：It is (identical with the organic solvent in step (1)) organic with alkaline with organic solvent
Solution, it is denoted as solution B；
OH in solution B-Molar concentration be 0.01~1.0mol/L；
(3) solution B that step (2) is configured is slowly dropped in solution A, remained during addition stirring and
Solution temperature is constant, obtains the solidliquid mixture containing blue precipitate；
(4) pure water is added in the solidliquid mixture containing blue precipitate that step (3) is obtained, maintenance temperature 60~
78 DEG C of more than 1min, now blue precipitate be gradually transformed into the CuO sediments of brown and/or black；
(5) the solidliquid mixture ethanol centrifuge washing 3~5 times containing CuO precipitations for being obtained step (4), finally will
Product heats after centrifuge washing dry 6~12h, obtain CuO nanometer rods.
Further, the organic solvent in step (1) and step (2) is ethanol, ethylene glycol, glycerine and N, N- dimethyl
One or more of mixtures in formamide.
Preferably, OH in solution B-Molar concentration and solution A in Cu2+Molar concentration rate be 10:1~1:1.
Preferably, in step (3), solution B is added drop-wise in solution A dropwise.
Further, the volume of pure water and the ratio between cumulative volume of organic solvent in step (1) and (2) are 1 in step (4):6
~6:1.
Preferably, centrifugal rotational speed is 7000~9000r/min in the step (5), centrifuges 15~30min every time.
Preferably, finally 6~12h will be dried at 50~80 DEG C of product after centrifuge washing.
The present invention has the advantages and positive effects of：The present invention develops one kind without using any surfactant and mould
The nanometer CuO powder process of plate agent, synthesized CuO are nanorod structure, and its diameter is less than 15nm, and entirely prepares
Journey is easy to operate, cost is cheap, has both solved nanoscale lower surface activating agent and the shortcomings that template is difficult to thoroughly remove,
Environment-friendly high-efficiency, industrial requirement simple to operate, being adapted to large-scale production are instantly catered to.
The present invention has the advantages and positive effects of：The preparation method for the CuO nanometer rods that the application provides, using liquid phase
Synthetic method, cost is low, and controllability is good, operability it is simple and convenient, by mantoquita species, reactant concentration, reaction temperature tune
Control, prepares purity height, the CuO nanometer rods of size uniform, and the CuO nanorod diameters prepared are less than 15nm.
The preparation method for the CuO nanometer rods that the application provides, without any surfactant and template, subsequent treatment letter
It is single, convenient, without removing surfactant and template in CuO, obtained CuO nanometer rods purity height, size uniform, to nanometer
The lifting of CuO performances is significant.
Brief description of the drawings
Transmission electron micrograph under Fig. 1 (a), the different amplification that (b) is CuO nanometer rods prepared by embodiment 1.
Fig. 2 is the transmission electron micrograph of CuO nanometer rods prepared by embodiment 2.
Embodiment
In order to be better understood from the present invention, the present invention is further retouched with reference to specific embodiments and the drawings
State.
Embodiment 1
A kind of preparation method of CuO nanometer rods, comprises the following steps：
(1)：0.029g copper nitrates are mixed with 30mL absolute ethyl alcohols, recycle ultrasonic vibration to obtain the pale blue of clear
Color solution, and the copper nitrate solution configured is heated to 75 DEG C under the conditions of magnetic agitation, it is denoted as solution A；
(2)：0.024g sodium hydroxides and 30mL absolute ethyl alcohols are configured to solution, are denoted as solution B；
(3)：The solution B that step (2) is configured is added dropwise in solution A, this process keeps magnetic agitation and maintained
Temperature obtains the solidliquid mixture containing blue precipitate at 75 DEG C；
(4)：Temperature is maintained at 75 DEG C, 30mL pure water is added to the consolidating containing blue precipitate that step (3) obtained
In liquid mixture, 15min is incubated, obtains the solidliquid mixture containing CuO precipitations；
(5)：The solidliquid mixture absolute ethyl alcohol centrifuge washing 5 times containing CuO precipitations that step (4) is obtained, turns
Fast 7000r/min, 25min is centrifuged every time, the product after centrifuge washing is finally dried into 6h at 80 DEG C, obtains CuO nanometer rods.
The TEM figures for the CuO nanometer rods that the present embodiment obtains are as shown in Figure 1.(a) and (b) is under distinct methods multiple in Fig. 1
Figure, it can be seen that obtained CuO nanometer rods length, even thickness, the diameter of CuO nanometer rods is less than 15nm.
Embodiment 2
A kind of preparation method of CuO nanometer rods, comprises the following steps：
(1)：1.870g copper nitrates are mixed with 100mL glycerine, recycle ultrasonic vibration to obtain the light blue molten of clarification
Liquid, and the copper nitrate solution configured is heated to 70 DEG C under the conditions of magnetic agitation, it is denoted as solution A；
(2)：0.560g potassium hydroxide and 50mL glycerine are configured to solution, are denoted as solution B；
(3)：The solution B that step (2) is configured is added dropwise in solution A, this process is kept stirring for being heated to 70 DEG C,
Obtain the solidliquid mixture containing blue precipitate；
(4)：Temperature is maintained at 70 DEG C, 50mL pure water is added to the consolidating containing blue precipitate that step (3) obtained
In liquid mixture, soaking time 20min, the solidliquid mixture containing CuO precipitations is obtained；
(5)：The solidliquid mixture absolute ethyl alcohol centrifuge washing 4 times containing CuO precipitations that step (4) is obtained, turns
Fast 8000r/min, 20min is centrifuged every time, the product after centrifuge washing is finally dried into 8h at 70 DEG C, obtains CuO nanometer rods.
The TEM figures for the CuO nanometer rods that the present embodiment obtains are as shown in Figure 1.It can be seen that obtained CuO nanometers
Rod length, even thickness, the diameter of CuO nanometer rods are less than 15nm.
Embodiment 3
A kind of preparation method of CuO nanometer rods of the present embodiment, comprises the following steps：
(1)：0.090g copper acetates are mixed with 50mL DMFs (DMF), recycle ultrasonic vibration to obtain
The light blue solution of clear, and the acetic acid copper solution configured is heated to 65 DEG C and insulation 10 under the conditions of magnetic agitation
Minute, it is denoted as solution A；
(2)：0.072g sodium hydroxides and 20mL DMF are configured to solution, are denoted as solution B；
(3)：The solution B that step (2) is configured is added dropwise in solution A, this process is kept stirring for being heated to 65 DEG C,
Obtain the solidliquid mixture containing blue precipitate；
(4)：Temperature is maintained at 65 DEG C, 70mL pure water is added to the consolidating containing blue precipitate that step (3) obtained
In liquid mixture, soaking time 40min, the solidliquid mixture containing CuO precipitations is obtained；
(5)：The solidliquid mixture absolute ethyl alcohol centrifuge washing 3 times containing CuO precipitations that step (4) is obtained, turns
Fast 8500r/min, 15min is centrifuged every time, the product after centrifuge washing is finally dried into 10h at 65 DEG C, obtains CuO nanometers
Rod.
Embodiment 4
A kind of preparation method of CuO nanometer rods of the present embodiment, comprises the following steps：
(1)：1.345g copper chlorides are mixed with 200mL ethylene glycol, recycle ultrasonic vibration to obtain the pale blue of clear
Color solution, and the copper chloride solution configured is heated to 78 DEG C under the conditions of magnetic agitation, it is denoted as solution A；
(2)：0.140g sodium hydroxides and 50mL ethylene glycol are configured to solution, are denoted as solution B；
(3)：The solution B that step (2) is configured is added dropwise in solution A, this process is kept stirring for being heated to 78 DEG C,
Obtain the solidliquid mixture containing blue precipitate；
(4)：Temperature is maintained at 78 DEG C, 750mL pure water is added to the consolidating containing blue precipitate that step (3) obtained
In liquid mixture, soaking time 10min, the solidliquid mixture containing CuO precipitations is obtained；
(5)：The solidliquid mixture absolute ethyl alcohol centrifuge washing 5 times containing CuO precipitations that step (4) is obtained, turns
Fast 8000r/min, 15min is centrifuged every time, the product after centrifuge washing is finally dried into 12h at 55 DEG C, obtains CuO nanometers
Rod.
Embodiment 5
A kind of preparation method of CuO nanometer rods of the present embodiment, comprises the following steps：
(1)：1.915g copper sulphate is mixed with 150mL absolute ethyl alcohols, recycles ultrasonic vibration to obtain the light of clear
Blue solution, and the copper-bath configured is heated to 60 DEG C under the conditions of magnetic agitation, it is denoted as solution A；
(2)：0.720g sodium hydroxides and 30mL absolute ethyl alcohols are configured to solution, are denoted as solution B；
(3)：The solution B that step (2) is configured is added dropwise in solution A, this process is kept stirring for being heated to 60 DEG C,
Obtain the solidliquid mixture containing blue precipitate；
(4)：Temperature is maintained at 60 DEG C, 1L pure water is added into the solid-liquid containing blue precipitate that (3) obtained mixes
In thing, soaking time 5min, the solidliquid mixture containing CuO precipitations is obtained；
(5)：The solidliquid mixture absolute ethyl alcohol centrifuge washing 5 times containing CuO precipitations that step (4) is obtained, turn
Fast 9000r/min, 20min is centrifuged every time, the product after centrifuge washing is finally dried into 7h at 75 DEG C, obtains CuO nanometer rods.
Embodiments of the invention are described in detail above, but the content is only presently preferred embodiments of the present invention,
It is not to be regarded as the practical range for limiting the present invention.All equivalent changes made according to the scope of the invention and improvement etc., all should
Still belong within this patent covering scope.
Claims (7)
- A kind of 1. preparation method of CuO nanometer rods, it is characterised in that：Comprise the following steps：(1) organic solution of cupric salt is prepared：The organic solution of cupric salt is prepared with organic solvent, makes Cu2+It is mole dense Spend for 0.001~0.1mol/L, and cupric salt solution is stirred and heated to 60~78 DEG C, be denoted as solution A；Described cupric salt is Cu (NO3)2、Cu(CH3COO)2、CuSO4、CuCl2In one or more of mixtures；(2) organic solution of alkaline is matched somebody with somebody：It is (identical with the organic solvent in step (1)) organic molten with alkaline with organic solvent Liquid, it is denoted as solution B；OH in solution B-Molar concentration be 0.01~1.0mol/L；(3) solution B that step (2) is configured is slowly dropped in solution A, stirring and solution is remained during addition It is temperature-resistant, obtain the solidliquid mixture containing blue precipitate；(4) pure water is added in the solidliquid mixture containing blue precipitate that step (3) is obtained, maintains 60~78 DEG C of temperature More than 1min, now blue precipitate be gradually transformed into the CuO sediments of brown and/or black；(5) the solidliquid mixture ethanol centrifuge washing 3~5 times containing CuO precipitations for being obtained step (4), finally will centrifugation Product heats after washing dry 6~12h, obtain CuO nanometer rods.
- 2. the preparation method of CuO nanometer rods according to claim 1, it is characterised in that：Step(1) organic solvent and in step (2) be one kind in ethanol, ethylene glycol, glycerine and N,N-dimethylformamide or Several mixtures.
- 3. the preparation method of CuO nanometer rods according to claim 1, it is characterised in that：OH in solution B-Molar concentration with Cu in solution A2+Molar concentration rate be 10:1~1:1.
- 4. the preparation method of CuO nanometer rods according to claim 1, it is characterised in that：In step (3), by solution B dropwise It is added drop-wise in solution A.
- 5. the preparation method of CuO nanometer rods according to claim 1 or 2, it is characterised in that：The body of pure water in step (4) Product is 1 with the ratio between cumulative volume of organic solvent in step (1) and (2):6~6:1.
- 6. the preparation method of CuO nanometer rods according to claim 1, it is characterised in that：Centrifugal rotational speed in the step (5) For 7000~9000r/min, 15~30min is centrifuged every time.
- 7. the preparation method of the CuO nanometer rods according to claim 1 or 6, it is characterised in that：Finally by after centrifuge washing 6~12h is dried at 50~80 DEG C of product.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109761262A (en) * | 2019-03-14 | 2019-05-17 | 东北大学 | A kind of preparation method and application of precious metal impregnation codope CuO nano material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102786075A (en) * | 2012-07-18 | 2012-11-21 | 西安交通大学 | Preparation method of flower-like nanometer copper oxide powder |
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- 2017-07-28 CN CN201710633070.4A patent/CN107344729A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102786075A (en) * | 2012-07-18 | 2012-11-21 | 西安交通大学 | Preparation method of flower-like nanometer copper oxide powder |
Non-Patent Citations (1)
| Title |
|---|
| L.-J. CHEN ET AL.: ""CuO NANOCRYSTALS IN THERMAL DECOMPOSITION OF AMMONIUM PERCHLORATE Stabilization, structural characterization and catalytic activities"", 《JOURNAL OF THERMAL ANALYSIS AND CALORIMETRY》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109761262A (en) * | 2019-03-14 | 2019-05-17 | 东北大学 | A kind of preparation method and application of precious metal impregnation codope CuO nano material |
| CN109761262B (en) * | 2019-03-14 | 2021-04-23 | 东北大学 | Preparation method and application of noble metal impregnation co-doping CuO nano material |
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