CN104841947A - Synthesis method of cable type silver chloride coated copper nano-structure - Google Patents
Synthesis method of cable type silver chloride coated copper nano-structure Download PDFInfo
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- CN104841947A CN104841947A CN201510215425.9A CN201510215425A CN104841947A CN 104841947 A CN104841947 A CN 104841947A CN 201510215425 A CN201510215425 A CN 201510215425A CN 104841947 A CN104841947 A CN 104841947A
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Abstract
The invention relates to a synthesis method of a cable type silver chloride coated copper nano-structure. The synthesis method comprises the following specific steps: firstly, solution preparation: preparing reaction substrates including a mixed solution of a copper salt, a reducing agent, a structure-directing agent, a surfactant solution and a silver salt solution; secondly, a synthesis method of a copper nano-wire: magnetically mixing the mixed solution containing the copper salt, the reducing agent and the structure-directing agent for a certain time at room temperature, and then transferring to an oil bath pan, insulating for a certain time at special temperature, cooling to room temperature after the completion of reaction, centrifuging, washing and collecting a sample to obtain a product; thirdly, silver chloride quantum dots: dripping the silver salt solution with certain concentration into the surfactant solution with certain solution, and magnetically stirring for a certain time to obtain a milky white solution; and fourthly, a synthesis method of a cable type silver chloride coated copper nano-wire: adding the copper nano-wire into the above milky white solution, and magnetically stirring for a certain time. The synthesis method of the cable type silver chloride coated copper nano-structure provided by the invention is simple in process, universal in preparation condition, stable in product morphology, high in purity and simple to process a product, thereby being applicable to medium-scale industrial production.
Description
Technical field
The invention belongs to technical field of inorganic nanometer material, particularly relate to the synthetic method of a kind of cable-type silver chlorate parcel copper nanostructured.
Background technology
Nanoscale science and technology be late 1980s produce one just in the new technology of fast development.So-called nanometer technology refers to unit---the nanoparticle with some molecules or atomic building, the science and technology of manufactured materials or microdevice.Nano structural material (at least 1 dimension (1D) yardstick is at 1 ~ 100nm) presents many character corresponding to main body phase material, causes the extensive concern of people.Along with the development of modern science and technology, the pattern research of nano structural material and preparation method there has also been large development.Nano effect comes from the restriction of potential well to electronics of nano-scale structure, thus achieves the control of the performances such as electricity, optics, magnetics and the thermoelectricity to solid.This field, in the development of recent two decades, achieves major progress in 0 dimension (OD) and 2 dimension (2D) nano structural material developments.As occurred, multiple method prepares quantum dot or the SQW of different materials, and can realize the good control of yardstick.Large quantity research, using quantum dot as system model, inquires into the change of the fundamental characteristics such as chemistry, physics with yardstick of material.Using quantum dot as active component, develop the nanodevice that many types can be used as cellular construction, as quantum dot laser, single-electronic transistor, mnemon body, sensor, optical detector and light emitting diode.2D nano structural material obtains extensive research in semiconductor applications, and molecular beam epitaxy trend technology more easily prepares 2D nano structural material.
In recent years, 1D nano structural material to be worth and potential technological applications is worth and becomes new study hotspot because it has important basic scientific research.1D nanostructured is research electrical conductivity and mechanical characteristic and the ideal system of relation between yardstick and Spatial Dimension, this for the node prepared in nanoscale electronic devices and photoelectron device and functional unit significant.There are some researches show, 1D nano structural material has many peculiar properties, as thermoelectricity capability coefficient and the lower laser threshold of superior mechanical toughness, high cold light efficiency, strengthening.Wherein, nano wire refers to that the anisotropy with comparatively wide aspect ratio (L/D ratio) is nanocrystalline, and generally its diameter is 1-200 nm, and length is tens microns.The spherical nanocrystalline characteristics such as physical property that cause because of varying topography have larger difference to nano wire with it.A major issue in 1D nano structural material research application how effectively to prepare 1D nanostructured by controlled method.Although the micro-shadow technology of senior nanometer, as electron beam lithography, the nearly technology such as probe modification and the micro-shadow of X-ray can prepare 1D nano structural material, these method preparation process are slow and cost is very high, cannot promote in actual applications.Therefore, research at present focuses mostly in preparing 1D nano structural material by chemical method, because these class methods can realize the control to nanometer dimension, cost is lower simultaneously, productive rate is higher.
In numerous 1D nano structural materials, metal nanometer line causes day by day to be paid close attention to widely.From German Gleiter since 1984 prepare the Fe nanometer particles of 6 nm first, in the world to the research mushroom development of nano metal, and make great progress.Wherein, copper nano material causes the concern of researcher day by day.Silver halide is widely used in manufacturing photo film, on hectograph and gummed paper. silver chlorate also has very important application in electrochemistry, silver monochlor(in)ate silver reference electrode not easily polarizes, thus more accurate data can be provided. the photosensitivity of silver halide and instability limit its application in photocatalysis, if can make silver halide under light illumination stable existence just can be applied to photocatalysis aspect. and the argent of nanoscale has stronger absorption in black light district, by adjusting the size of argent, shape and the environment residing for nano particle can make its absorption spectrum generation red shift.In theory, silver nano-grain can be utilized to strengthen the absorption of catalysis material to sunshine.In this experiment, copper and silver chlorate are carried out effective compound, form the network structure of Cu/AgCl, first, due to the close contact of metallic copper and silver chlorate, the electronic energy produced in system is more easily delivered in metallic silver particles, effectively facilitate being separated and then improve quantum efficiency of electronics and hole, ensure that the stability of system; Secondly, the network structure of this novelty has larger specific area, can provide more how light-catalysed avtive spot, improves catalytic efficiency; Again, the nano cable structure of Cu@AgCl has expanded the response of system to visible ray effectively, makes it have very strong absorption at whole visible region, substantially increases the utilization rate to sunshine.This method has been widened and has been strengthened catalysis material to the approach of visible absorption by metal surface plasma resonance body effect, and then improves the performance of catalysis material.
Summary of the invention
The object of this invention is to provide a kind of synthetic method of cable-type silver chlorate parcel copper nanostructured.
To achieve these goals, technical scheme of the present invention is as follows:
The synthetic method of the cable-type silver chlorate parcel copper nanostructured that the present invention proposes, concrete steps are as follows:
(1) configuration of solution
Prepare reaction substrate mixed solution respectively, surfactant solution and silver salt solution; Wherein: described reaction substrate mixed solution is made up of mantoquita, reducing agent and structure directing agent, the mol ratio of mantoquita, reducing agent and structure directing agent is 1:4:6;
(2) synthetic method of copper nano-wire
Reaction substrate mixed solution is stirred 12h at normal temperature condition lower magnetic force, is then transferred in oil bath pan, be incubated 6 hours in the oil bath pan at 110 DEG C of temperature, reaction terminates, and is cooled to room temperature, is undertaken centrifugal by sample, and washing, collects to obtain copper nano-wire;
(3) quantum dot of silver chlorate
Dropwise joined in surfactant solution by the silver salt solution that step (1) obtains, normal temperature condition lower magnetic force stirs 30min, obtains milky white solution;
(4) synthetic method of silver chlorate supported copper nano wire
Joined by copper nano-wire in the milky white solution of step (3) gained, normal temperature condition lower magnetic force stirs 12 hours, and reaction terminates, and is cooled to room temperature, is undertaken centrifugal by sample, and washing is dry, collects, obtains product.
In the present invention, described in step (1), step (2), step (3) and step (4), solvent is deionized water.
In the present invention, described mantoquita is Copper dichloride dihydrate, and its concentration is 0.01mol/L.
In the present invention, described reducing agent is glucose, and its concentration is 0.04mol/L.
In the present invention, described structure directing agent is cetylamine, and its concentration is 0.06mol/L.
In the present invention, described surfactant is DTAC, and its concentration is 0.121mol/L.
In the present invention, described silver salt is silver nitrate, and its concentration is 0.101mol/L.
In the present invention, step (2) and the described washing of step (4) use ethanol and deionized water washed product respectively.
In the present invention, step (4) described drying is dry 10h in 60 DEG C of vacuum drying chambers.
Owing to adopting such scheme, the present invention has following beneficial effect:
1, present invention achieves and utilize common mantoquita and nitrate to be presoma, heated the composite having synthesized Cu@AgCl network structure first by oil bath.
2, the pattern of method of the present invention to product has very high control.
3, the present invention adopts simple inorganic salts as reactant, has very strong versatility.
4, the product that prepared by the present invention has the good Photocatalytic Degradation Property to organic pollution, as high-performance optical catalyst, can have comparatively vast potential for future development and application space.
5, technique of the present invention is simple, and preparation condition is general, and product morphology is stable, purity is high, and product process is convenient succinct, is suitable for medium-scale industrial production.
6, method of the present invention has mild condition, homogeneous heating, efficient energy-saving, is easy to the features such as control.
Accompanying drawing explanation
Fig. 1 is the SEM photo of the intermediate product obtained under the multiple of 50nm in embodiment 1.
Fig. 2 is the SEM photo of the product obtained under the multiple of 50nm in embodiment 1.
Fig. 3 is the TEM photo of the product obtained under the multiple of 500nm in embodiment 1.
Fig. 4 is the XRD collection of illustrative plates of products therefrom in embodiment 1.
Fig. 5 is the EDS collection of illustrative plates of products therefrom in embodiment 1.
Fig. 6 is the SEM photo of the intermediate product obtained under the multiple of 200nm in embodiment 2.
Fig. 7 is the SEM photo of the intermediate product obtained under the multiple of 500nm in embodiment 3.
Detailed description of the invention
Below in conjunction with accompanying drawing illustrated embodiment, the present invention is further detailed explanation.
Embodiment 1
The first step: take 0.16g DTAC (DTAC) and 0.086g AgNO respectively
3be placed in the 25ml reaction bulb that label is respectively B and C respectively, add 5ml deionized water and magneton dissolving respectively, by AgNO
3dropwise joins in DTAC solution, and magnetic agitation 30min, obtains milky white solution.Take 0.0220g CuCl respectively
22H
2o, 0.1846g cetylamine (HAD), 0.0754g glucose is placed in the 25ml reaction bulb that label is A, and add 10ml deionized water and magneton, normal temperature magnetic agitation 12h is to being dissolved as blue solution.
Second step: blue solution be fixed on iron stand, be placed in oil bath pan, open oil bath pan switch, set temperature is 110 DEG C, and opens magnetic agitation.
3rd step: wait oil bath pan to reach set temperature and stablize, magnetic agitation reaction 6h, solution becomes brick-red.Close oil bath pan, and reaction bulb is shifted out liquid level, be cooled to room temperature, respectively wash by absolute ethyl alcohol and deionized water and once obtain brick-red solid.
4th step: brick-red solid is joined in milky white solution, add magneton, normal temperature magnetic agitation.
5th step: reaction 12h, with absolute ethyl alcohol and deionized water washing several, is placed in vacuum drying chamber dry.
Fig. 1 is the SEM photo of the intermediate product obtained under the multiple of 50nm in embodiment 1; Fig. 2 is the SEM photo of the product obtained under the multiple of 50nm in embodiment 1; Fig. 3 is the TEM photo of the product obtained under the multiple of 500nm in embodiment 1; Fig. 4 is the XRD collection of illustrative plates of embodiment 1 products therefrom, and the existing AgCl in compound is described, has again Cu to exist.Fig. 5 is the EDS collection of illustrative plates of embodiment 1 products therefrom.
Embodiment 2
The first step: take 0.16g DTAC (DTAC) and 0.086g AgNO respectively
3be placed in the 25ml reaction bulb that label is respectively B and C respectively, add 5ml deionized water and magneton dissolving respectively, by AgNO
3dropwise joins in DTAC solution, and magnetic agitation 30min, obtains milky white solution.Take 0.0880g CuCl respectively
22H
2o, 0.7384g cetylamine (HAD), 0.3016g glucose is placed in the 25ml reaction bulb that label is A, and add 10ml deionized water and magneton, normal temperature magnetic agitation 12h is to being dissolved as blue solution.
Second step: blue solution be fixed on iron stand, be placed in oil bath pan, open oil bath pan switch, set temperature is 110 DEG C, and opens magnetic agitation.
3rd step: wait oil bath pan to reach set temperature and stablize, magnetic agitation reaction 6h, solution becomes brick-red.Close oil bath pan, and reaction bulb is shifted out liquid level, be cooled to room temperature, respectively wash by absolute ethyl alcohol and deionized water and once obtain brick-red solid.
4th step: brick-red solid is joined in milky white solution, add magneton, normal temperature magnetic agitation.
5th step: reaction 12h, with absolute ethyl alcohol and deionized water washing several, is placed in vacuum drying chamber dry.
Fig. 6 is the SEM photo of the product obtained under the multiple of 200nm in embodiment 2.As can be seen from picture, still can form the nano cable structure of Cu/AgCl with this understanding, just the silver chlorate particle of load is less.
Embodiment 3
The first step: take 0.16g DTAC (DTAC) and 0.086g AgNO respectively
3be placed in the 25ml reaction bulb that label is respectively B and C respectively, add 5ml deionized water and magneton dissolving respectively, by AgNO
3dropwise joins in DTAC solution, and magnetic agitation 30min, obtains milky white solution.Take 0.440g CuCl respectively
22H
2o, 3.692g cetylamine (HAD), 1.508g glucose is placed in the 25ml reaction bulb that label is A, and add 10ml deionized water and magneton, normal temperature magnetic agitation 12h is to being dissolved as blue solution.
Second step: blue solution be fixed on iron stand, be placed in oil bath pan, open oil bath pan switch, set temperature is 110 DEG C, and opens magnetic agitation.
3rd step: wait oil bath pan to reach set temperature and stablize, magnetic agitation reaction 6h, solution becomes brick-red.Close oil bath pan, and reaction bulb is shifted out liquid level, be cooled to room temperature, respectively wash by absolute ethyl alcohol and deionized water and once obtain brick-red solid.
4th step: brick-red solid is joined in milky white solution, add magneton, normal temperature magnetic agitation.
5th step: reaction 12h, with absolute ethyl alcohol and deionized water washing several, is placed in vacuum drying chamber dry.
Fig. 7 is the SEM photo of the product obtained under the multiple of 500nm in embodiment 3.As can be seen from picture, still can form the nano cable structure of Cu@AgCl with this understanding, just the silver chlorate particle of load is more rare.
Above-mentioned is can understand and apply the invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to embodiment here, the amendment made when not departing from category of the present invention is all within protection scope of the present invention.
Claims (9)
1. a synthetic method for cable-type silver chlorate parcel copper nanostructured, is characterized in that concrete steps are as follows:
(1) configuration of solution
Prepare reaction substrate mixed solution respectively, surfactant solution and silver salt solution; Wherein: described reactant mixed solution is made up of mantoquita, reducing agent and structure directing agent, the mol ratio of mantoquita, reducing agent and structure directing agent is 1:4:6;
(2) synthetic method of copper nano-wire
Reaction substrate mixed solution is stirred 12h at normal temperature condition lower magnetic force, is then transferred in oil bath pan, be incubated 6 hours in the oil bath pan at 110 DEG C of temperature, reaction terminates, and is cooled to room temperature, is undertaken centrifugal by sample, and washing, collects to obtain copper nano-wire;
(3) quantum dot of silver chlorate
Dropwise joined in surfactant solution by the silver salt solution that step (1) obtains, normal temperature condition lower magnetic force stirs 30min, obtains milky white solution;
(4) synthetic method of silver chlorate supported copper nano wire
Joined by copper nano-wire in the milky white solution of step (3) gained, normal temperature condition lower magnetic force stirs 12 hours, and reaction terminates, and is cooled to room temperature, is undertaken centrifugal by sample, and washing is dry, collects, obtains product.
2. the method for a kind of synthesizing chlorinated silver-colored supported copper nano wire according to claim 1, is characterized in that: described in step (1), step (2), step (3) and step (4), solvent is deionized water.
3. the method for a kind of synthesizing chlorinated silver-colored supported copper nano wire according to claim 1, it is characterized in that: described mantoquita is Copper dichloride dihydrate, its concentration is 0.01mol/L.
4. the method for a kind of synthesizing chlorinated silver-colored supported copper nano wire according to claim 1, it is characterized in that: described reducing agent is glucose, its concentration is 0.04mol/L.
5. the method for a kind of synthesizing chlorinated silver-colored supported copper nano wire according to claim 1, it is characterized in that: described structure directing agent is cetylamine, its concentration is 0.06mol/L.
6. the method for a kind of synthesizing chlorinated silver-colored supported copper nano wire according to claim 1, it is characterized in that: described surfactant is DTAC, its concentration is 0.121mol/L.
7. the method for a kind of synthesizing chlorinated silver-colored supported copper nano wire according to claim 1, it is characterized in that: described silver salt is silver nitrate, its concentration is 0.101mol/L.
8. the method for a kind of synthesizing chlorinated silver-colored supported copper nano wire according to claim 1, is characterized in that: step (2) and the described washing of step (4) use ethanol and deionized water washed product respectively.
9. the method for a kind of synthesizing chlorinated silver-colored supported copper nano wire according to claim 1, is characterized in that: step (4) described drying is dry 10h in 60 DEG C of vacuum drying chambers.
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