CN105712741A - Preparation method of copper oxide nanowires - Google Patents
Preparation method of copper oxide nanowires Download PDFInfo
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- CN105712741A CN105712741A CN201511010291.3A CN201511010291A CN105712741A CN 105712741 A CN105712741 A CN 105712741A CN 201511010291 A CN201511010291 A CN 201511010291A CN 105712741 A CN105712741 A CN 105712741A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5072—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with oxides or hydroxides not covered by C04B41/5025
- C04B41/5074—Copper oxide or solid solutions thereof
- C04B41/5075—Copper oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/72—Copper
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
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- C—CHEMISTRY; METALLURGY
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/0081—Uses not provided for elsewhere in C04B2111/00 as catalysts or catalyst carriers
Abstract
The invention provides a preparation method of copper oxide nanowires. The preparation method includes: preparing a bivalent copper salt solution and a complexing agent solution, adding complexing agent into the bivalent copper salt solution, evenly stirring to obtain bivalent copper salt mixed solution, slowly adding a sodium hydroxide solution into the bivalent copper salt mixed solution under an intense stirring condition to form a mixture solution, transferring the mixture solution into a reaction kettle for reaction to obtain two-dimensional material loaded with nanostructure copper oxide, wherein reaction base material graphene paper is adhered to the inner wall of the reaction kettle. The preparation method has the advantages that the method is short in reaction cycle and high in efficiency, and the generation speed of the copper oxide is controlled by using the appropriate complexing agent.
Description
Technical field
The present invention relates to a nanometer new material processing and manufacturing technical field, the preparation method being specifically related to a kind of cupric oxide nano line.
Background technology
The common methods preparing supported copper oxide nano wire (by cupric oxide nano linear load to planar substrate) at present has template-chemical precipitation method (such as patent CN201510061151.2), template-thermal oxidation method (such as CN200910038947.0), thermal oxidation method (such as patent CN200610034006.6, CN201110094054.5), plasma bombardment method (such as patent CN201210264695.5), said method preparation technology complex or to process conditions require higher.Such as, in above-mentioned thermal oxidation method, (CN201110094054.5) needs first to adopt magnetron sputtering method that metallic copper deposits to formation metal copper film in substrate in high vacuum, is then annealed under atmospheric atmosphere by the thin film prepared and namely obtains nanowire array of copper oxide thin film；For another example, in above-mentioned plasma bombardment method (such as patent CN201210264695.5), needing first by thermal oxide, Copper thin film to be generated CuO film, CuO film is carved into nano-wire array by the method-plasma bombardment method then passing through physics.For another example; template-thermal oxidation method that patent CN200910038947.0 reports; the method is first to prepare multilayer transition layer, metal film and protective layer successively on substrate; then pass through photoetching method and optionally expose metallic film surface; finally this surface is placed under the atmosphere containing oxygen and heats, it is achieved the growth of its oxide nano thread.Generally, these methods mostly relate to physical treatment course (such as photoetching in preparation process, sputtering, plasma bombardment etc.), therefore preparation process is complex, process costs is higher, and currently used solution chemical processes is easily achieved copper oxide nanometer particle deposition on planar substrate thus obtaining supported copper oxide nano material, but use solution chemical processes to be deposited on planar substrate by cupric oxide nano line to obtain supported copper oxide nano wire then highly difficult, because nano wire is longer, it is sterically hindered also much larger than spherical nanoparticle, it is not easy to be deposited on base material, therefore, the method of the many employings of existing method (or part adopts) physics realizes cupric oxide nano line deposition on base material.
Summary of the invention
The technical problem to be solved is to provide, for above-mentioned the deficiencies in the prior art, the two dimensional surface substrate support cupric oxide nano line preparation method that a kind of production cost is low, reaction time is short, efficiency is high.
The present invention solves that the technical scheme that the problems referred to above adopt is:
The preparation method that the present invention provides a kind of cupric oxide nano line, comprises the following steps:
(1) take 2～200mmol cupric salt be dissolved in 40mL water and stir formation cupric salt solution, take a certain amount of chelating agent formation enveloping agent solution that stirs soluble in water, adding chelating agent in described cupric salt solution to stir formation cupric salt mixed solution, the mol ratio of described chelating agent and described cupric salt is 1:1～4:1；
(2) take 25～300mmol sodium hydroxide to be dissolved in 40mL water and form sodium hydroxide solution；
(3) described sodium hydroxide solution is slowly added in described cupric salt mixed solution to stir formation mixture solution under intense agitation；
(4) described mixture solution is proceeded to inwall post reaction base material reactor in react, on described graphite paper base material, uniform deposition has the copper oxide of nanostructured, and on described graphite paper base material, form nanostructured CuO film, thus obtaining being loaded with the two-dimensional material of nanostructured CuO film.
Further, step (1) described cupric salt is CuSO4·5H2O、CuCl2With Cu (NO3)2In one or more, described chelating agent is one or more in EDTA, sodium citrate, sodium tartrate, ethylenediamine, salicylic acid, HQS and triethylene tetramine.
Further, base material described in step (4) is graphite paper, and described base material is the base material of long 12cm, wide 5cm.
Further, the mixture solution response time in a kettle. described in step (4) is 1～6h, and temperature is 100～180 DEG C.
The beneficial effects of the present invention is:
The preparation method one-step method of a kind of cupric oxide nano line provided by the present invention, the reagent used is cheap reagent, reaction time is short, it is 1 hour the soonest, in addition, owing to this method employs suitable chelating agent, these chelating agent can with cupric salt complexation thus controlling the generating rate of copper oxide, the copper oxide nanocrystal generated is made to have preferred growth orientation thus to form some aspherical with specific morphology nanocrystalline, therefore, the basic component units of the copper oxide prepared by this method aspherical or spherical particle, but there is the nano wire of special shape, in addition, graphite paper conductivity is high, copper oxide nano material is loaded to above graphite paper as the catalyst used time, be conducive to the separation of charge of catalyst, thus reaching higher catalytic efficiency.
Accompanying drawing explanation
The graphite paper that Fig. 1 is prepared in embodiment 1 supports the XRD spectra of cupric oxide nano line；
The graphite paper that Fig. 2 is prepared in embodiment 1 supports the low power SEM picture of cupric oxide nano line；
The graphite paper that Fig. 3 is prepared in embodiment 1 supports the high power SEM picture of cupric oxide nano line；
The graphite paper that Fig. 4 is prepared in embodiment 1 supports the design sketch of the catalyzing hydrogen peroxide degraded Congo red of cupric oxide nano line；
Graphite paper prepared in Fig. 5 embodiment 1 supports total organic carbon (TOC) the clearance design sketch of the catalyzing hydrogen peroxide degraded Congo red of cupric oxide nano line.
Detailed description of the invention
Embodiments of the present invention are specifically illustrated below in conjunction with accompanying drawing; these embodiments be only given for illustrative purposes; limitation of the invention can not be interpreted as; and explanation only for reference including accompanying drawing uses; do not constitute the restriction to scope of patent protection of the present invention; because without departing from the spirit and scope of the present invention, it is possible to the present invention is carried out many changes.
Embodiment 1
Take 2mmolCuSO4·5H2O is dissolved in 20mL water and forms CuSO4·5H2O solution, the chelating agent such as triethylene tetramine taking 4mmol is dissolved in 20mL water and forms enveloping agent solution, by CuSO4·5H2O solution, enveloping agent solution is mixed and stirred for being formed uniformly mixed solution, then take the sodium hydroxide solution that the 40mL concentration prepared is 5mol/L and be added dropwise over above-mentioned mixed solution, stirring, finally give reactant liquor and proceed in reactor, by what cut, long 12cm, the graphite paper of wide 5cm is rolled into cylinder and is close to the inwall of reactor, react 3 hours under 180 DEG C of conditions, on graphite paper base material, uniform deposition has the copper oxide of nanostructured, and on described graphite paper base material, form nanostructured CuO film, thus obtaining being loaded with the two-dimensional material of nanostructured CuO film.
It is analyzed the material on base material finding, load material nanostructured CuO film on base material is copper oxide, cupric oxide nano line prepared by the present embodiment 1 is analyzed, as it is shown in figure 1, the graphite paper that Fig. 1 (a) is prepared in embodiment 1 supports the XRD spectra of cupric oxide nano line；B () is the XRD spectra of graphite paper base material, in figure, curve (b) is in 2 θ=26.8 °, 54.6 ° and 87.4 ° of places go out peak, corresponding is rhombus crystalline phase graphite (PDF#75-2078), curve (a) except above three peak also in 2 θ=36.8 °, 42.7 °, 61.8 ° and 74.1 ° of places go out peak, these four peaks correspondence respectively is face-centered cubic crystal formation copper oxide (111), (200), and (311) crystal face (220), (PDF#78-0428), from Fig. 2 and Fig. 3, find out that on graphite paper, the diameter of the cupric oxide nano line of deposition is 50-150 nanometer, length is 2-3 micron, and growth shape is very regular, degree of crystallinity is higher, as can be seen from Figure 4 when reacted between be 36min, the degradation rate of Congo red can reach 97.5%.
As can be seen from Figure 5 when reacted between be 80min, total organic carbon (TOC) clearance of Congo red can reach 77%, comprehensive analyze prepared graphite paper and supports cupric oxide nano line and have good physics, chemical property.
The preparation method of a kind of cupric oxide nano line provided by the present invention is one-step method, the reagent used is cheap reagent, preparation cost is low, reaction time is short, it is 1 hour the soonest, greatly improve preparation efficiency, in addition, owing to this method employs suitable chelating agent, these chelating agent can with cupric salt complexation thus controlling the generating rate of copper oxide, the copper oxide nanocrystal generated is made to have preferred growth orientation thus to form some aspherical with specific morphology nanocrystalline, therefore, the basic component units of the CuO film prepared by this method aspherical or spherical particle, but there is the nanocrystal of special shape, such as nano wire etc..
Embodiment 2
Take 0.4molCu (NO3)2It is dissolved in 40mL water and forms Cu (NO3)2Solution, the salicylic acid stirring and dissolving adding 0.8mol forms salicylic acid solution in 40mL water, by Cu (NO3)2The stirring mixing of solution, salicylic acid solution, then take the sodium hydroxide solution that 200mL concentration is 20mol/L and be added dropwise over above-mentioned mixed solution, stirring, finally give reactant liquor and proceed in reactor, the graphite paper of 6cm that cut, long, wide 1cm is rolled into cylinder and is close to the inwall of reactor, react 8 hours at 120 DEG C, on graphite paper base material, uniform deposition has the copper oxide of nanostructured, and on described graphite paper base material, form nanostructured copper oxide, thus obtaining being loaded with the two-dimensional material of nanostructured CuO film.
Embodiment 3
Take 10molCuCl2It is dissolved in 40mL water and forms CuCl2Solution, the sodium tartrate stirring and dissolving adding 10mol forms sodium tartrate solution in 40mL water.By CuCl2The stirring mixing of solution, sodium tartrate solution, then takes the sodium hydroxide solution that 200mL concentration is 20mol/L and is added dropwise over above-mentioned mixed solution, stirring.Finally give reactant liquor and proceed in reactor, the graphite paper of 6cm that cut, long, wide 2cm is rolled into cylinder and is close to the inwall of reactor, react 6 hours at 160 DEG C, on graphite paper base material, uniform deposition has the copper oxide of nanostructured, and on described graphite paper base material, form nanostructured copper oxide, thus obtaining being loaded with the two-dimensional material of nanostructured CuO film.
Embodiment 4
Take 0.4molCu (NO3)2It is dissolved in 40mL water and forms Cu (NO3)2Solution, the ethanolamine stirring and dissolving adding 0.8mol forms ethanolamine solutions in 40mL water.By Cu (NO3)2The stirring mixing of solution, ethanolamine solutions, then take the sodium hydroxide solution that 200mL concentration is 20mol/L and be added dropwise over above-mentioned mixed solution, stirring, finally give reactant liquor and proceed in reactor, the graphite paper of 12cm that cut, long, wide 8cm is rolled into cylinder and is close to the inwall of reactor, react 8 hours at 120 DEG C, on graphite paper base material, uniform deposition has the copper oxide of nanostructured, and on described graphite paper base material, form nanostructured copper oxide, thus obtaining being loaded with the two-dimensional material of nanostructured CuO film.
Embodiment 5
Take 0.1molCuCl2It is dissolved in 40mL water and forms CuCl2Solution, the HQS stirring and dissolving adding 0.2mol forms HQS solution in 40mL water, by CuCl2Solution, HQS solution stirring mix, then take the sodium hydroxide solution that 10mL concentration is 20mol/L and be added dropwise over above-mentioned mixed solution, stirring, finally give reactant liquor and proceed in reactor, the graphite paper of 6cm that cut, long, wide 6cm is rolled into cylinder and is close to the inwall of reactor.Reacting 6 hours at 140 DEG C, on graphite paper base material, uniform deposition has the copper oxide of nanostructured, and forms nanostructured copper oxide on described graphite paper base material, thus obtaining being loaded with the two-dimensional material of nanostructured CuO film
Above-described embodiment is the present invention preferably embodiment; but embodiments of the present invention are also not restricted to the described embodiments; the change made under other any spirit without departing from the present invention and principle, modification, replacement, combination, simplification; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (4)
1. the preparation method of a cupric oxide nano line, it is characterised in that comprise the following steps:
(1) take 2～200mmol cupric salt be dissolved in 40mL water and stir formation cupric salt solution, take a certain amount of chelating agent formation enveloping agent solution that stirs soluble in water, adding enveloping agent solution in described cupric salt solution to stir formation cupric salt mixed solution, the mol ratio of described chelating agent and described cupric salt is 1:1～4:1；
(2) take 25～300mmol sodium hydroxide to be dissolved in 40mL water and form sodium hydroxide solution；
(3) described sodium hydroxide solution is slowly added in described cupric salt mixed solution to stir formation mixture solution under intense agitation；
(4) described mixture solution proceeds to inwall post in the reactor of graphite paper base material and react, on described graphite paper base material, uniform deposition has the copper oxide of nanostructured, and on described graphite paper base material, form nanostructured CuO film, thus obtaining being loaded with the two-dimensional material of nanostructured CuO film.
2. the preparation method of a kind of cupric oxide nano line according to claim 1, it is characterised in that: step (1) described cupric salt is CuSO4·5H2O、CuCl2With Cu (NO3)2In one or more, described chelating agent is one or more in EDTA, sodium citrate, sodium tartrate, ethylenediamine, salicylic acid, HQS and triethylene tetramine.
3. the preparation method of a kind of cupric oxide nano line according to claim 1, it is characterised in that: base material described in step (4) is graphite paper, and described base material is the base material of long 12cm, wide 5cm.
4. the preparation method of a kind of cupric oxide nano line according to claim 1, it is characterised in that: the mixture solution response time in a kettle. described in step (4) is 1～6h, and temperature is 100～180 DEG C.
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| CN201511010291.3A CN105712741A (en) | 2015-12-25 | 2015-12-25 | Preparation method of copper oxide nanowires |
| PCT/CN2016/111953 WO2017107999A1 (en) | 2015-12-25 | 2016-12-24 | Method for preparing copper oxide nanowire |
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| CN201511010291.3A CN105712741A (en) | 2015-12-25 | 2015-12-25 | Preparation method of copper oxide nanowires |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107555466A (en) * | 2017-09-21 | 2018-01-09 | 华中农业大学 | A kind of preparation method of copper oxide nano fiber |
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| CN114318847A (en) * | 2021-12-21 | 2022-04-12 | 上海应用技术大学 | Carbon fiber composite material loaded with oxygen-deficient copper oxide and preparation method and application thereof |
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| CN103030169A (en) * | 2012-12-26 | 2013-04-10 | 中北大学 | Shape-controlled preparation method of nanometer copper oxide |
| CN103084581A (en) * | 2013-01-08 | 2013-05-08 | 河南大学 | Preparation method for copper nanowire |
| CN104030341A (en) * | 2014-06-11 | 2014-09-10 | 电子科技大学 | Preparation method of copper oxide nanomaterial |
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| CN103253672B (en) * | 2013-05-20 | 2014-11-26 | 浙江理工大学 | Preparation method of silicon carbide nanowire thin film based on hydrogen production by photoelectric catalytic decomposition of water |
| CN103352132A (en) * | 2013-07-05 | 2013-10-16 | 浙江大学 | Copper-nickel nanowire and preparation method thereof |
| CN103464775A (en) * | 2013-08-24 | 2013-12-25 | 四川大学 | Method for adopting magnetic-field self-assembling method to prepare cobalt nanowire |
| CN104493195B (en) * | 2014-12-05 | 2017-04-12 | 北京化工大学 | Amorphous-state copper-platinum alloy nanotube and preparation method thereof |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060090597A1 (en) * | 2004-10-29 | 2006-05-04 | Goia Dan V | Polyol-based method for producing ultra-fine metal powders |
| CN102251278A (en) * | 2011-05-31 | 2011-11-23 | 常州大学 | Controllable preparation method of monocrystal copper nanowires |
| CN103030169A (en) * | 2012-12-26 | 2013-04-10 | 中北大学 | Shape-controlled preparation method of nanometer copper oxide |
| CN103084581A (en) * | 2013-01-08 | 2013-05-08 | 河南大学 | Preparation method for copper nanowire |
| CN104030341A (en) * | 2014-06-11 | 2014-09-10 | 电子科技大学 | Preparation method of copper oxide nanomaterial |
| CN104176763A (en) * | 2014-07-22 | 2014-12-03 | 惠州学院 | Special-structure nano copper oxide film, and preparation method and application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107555466A (en) * | 2017-09-21 | 2018-01-09 | 华中农业大学 | A kind of preparation method of copper oxide nano fiber |
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