CN103274443A - Quadrangular leaf-shaped Cu2O-ZnO composite nano-structural semiconductor material, and preparation method thereof - Google Patents
Quadrangular leaf-shaped Cu2O-ZnO composite nano-structural semiconductor material, and preparation method thereof Download PDFInfo
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- CN103274443A CN103274443A CN2013101412593A CN201310141259A CN103274443A CN 103274443 A CN103274443 A CN 103274443A CN 2013101412593 A CN2013101412593 A CN 2013101412593A CN 201310141259 A CN201310141259 A CN 201310141259A CN 103274443 A CN103274443 A CN 103274443A
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Abstract
The invention discloses a quadrangular leaf-shaped Cu2O-ZnO composite nano-structural semiconductor material, comprising a silicon wafer substrate and a quadrangular leaf-shaped Cu2O-ZnO composite nano-structure grown on the silicon wafer substrate, wherein the Cu2O-ZnO composite nano-structure is composed of Cu2O microparticles and ZnO nanoparticles; the Cu2O microparticles have a quadrangular leaf-shaped structure; and the ZnO nanoparticles covers the surface of the Cu2O microparticles. The invention also discloses a preparation method for the quadrangular leaf-shaped Cu2O-ZnO composite nano-structural semiconductor material. The preparation method is simple in operations, and efficiency of light energy utilization of the obtained Cu2O-ZnO hetero nanostructure is significantly increased.
Description
Technical field
The invention belongs to photoelectron material, semiconductor material and device technology field, be specifically related to a kind of by the lobate Cu of four hornbeams
2The Cu that O micron particle and ZnO nano particle structure form
2O-ZnO composite nanostructure semiconductor material, and stepwise synthesis Cu
2Behind O micron particle and the ZnO nano particle with the two preparation method who is combined with each other.
Background technology
Cu
2O is widely used in solar cell, utilizes sunlight hydrolysis liberation of hydrogen, Li ionization cell and utilizes visible light degraded organic contamination etc. as a kind of common direct band gap p-type semi-conductor.ZnO is because its direct band gap, broad stopband (3.3eV, the near-ultraviolet light at corresponding about 380nm place), big relatively exciton binding energy (60meV), high carrier mobility and cheap prepares advantages such as simple, be widely used in solar cell, gas sensor, fields such as feds.
There have been some scientists to carry out Cu
2The research of O-ZnO base heterojunction solar cell application aspect.Yet, because Cu
2The lattice mismatch of O and ZnO, simultaneously, because Cu
2O has caused common VLS technology and hydrothermal method can not realize Cu in airborne relative instability below 1000 ℃
2Synthesizing of O-ZnO base hetero nano structure.Present synthetic Cu
2What O-ZnO base hetero nano structure adopted mostly is to electroplate, electrochemical synthesis or sputtering technology, and synthetic heterogeneous interface mostly is slab construction.This can cause the right defectives such as high recombination rate of carrier mobility curtailment and light induced electron-hole, thereby directly influences the solar energy utilising efficiency of heterojunction system.
Therefore, need a kind of easy Cu badly
2The preparation method of O-ZnO composite nanostructure and have the more Cu of high-light-energy utilization ratio
2The O-ZnO hetero nano structure.
Summary of the invention
The purpose of this invention is to provide the lobate Cu of a kind of four hornbeams
2O-ZnO composite nanostructure and preparation method thereof.
Cu provided by the present invention
2The O-ZnO composite nanostructure is by the lobate Cu of four hornbeams
2O micron particle and ZnO nano particle structure are composited under the booster action of poly-acetimide, Cu
2O matrix size is shaped as the lobate micron particle of four hornbeams generally at 1.5～3 μ m, and its surface recombination has the ZnO nano particle, and particle diameter is at 20～40nm.Among the present invention, Cu
2The O micron particle has four hornbeam foliation structures, and particularly, this structure is to be extended by the mutually perpendicular directions of four of middle mind-sets, is four horn shapes, and its surface presents the vein structure of similar leaf, so it is lobate to be called four hornbeams.This structure is of a size of 1.5～3 μ m in the length and width direction.
The present invention proposes the lobate Cu of a kind of four hornbeams
2O-ZnO composite nanostructure semiconductor material comprises silicon chip substrate, and is grown in the lobate Cu of four hornbeams on the described silicon chip
2The O-ZnO composite nanostructure.Wherein, described Cu
2The O-ZnO composite nanostructure is by Cu
2O micron particle and ZnO nano particle are formed, described Cu
2The O micron particle has four hornbeam foliation structures, and described ZnO nano particle covers described Cu
2O micron particle surface.Wherein, described Cu
2O micron particle central position has depression, grows the angle of the structure of foliated lamellar by described recess to mutually perpendicular four direction, and its surface has the tree leaf vein laminate structure.That is Cu,
2The O micron particle is extended by four mutually perpendicular directions of middle mind-set, be four horn shapes, and its surface presents the vein structure of similar leaf.
The lobate Cu of the present invention four hornbeams
2In the O-ZnO composite nanostructure semiconductor material, described Cu
2The O micron particle is of a size of 1.5～3 μ m in the length and width direction, and described ZnO nano particle diameter is 20～40nm.
The lobate Cu of the present invention four hornbeams
2In the O-ZnO composite nanostructure semiconductor material, utilize hydrothermal synthesis method synthetic Cu respectively
2O micron particle and ZnO nano particle make described ZnO nano particle be compounded in Cu equably with polymine as aid in material
2On the O micron particle, obtain the lobate Cu of described four hornbeams
2O-ZnO composite nanostructure semiconductor material.
The present invention also provides a kind of four hornbeams lobate Cu
2The preparation method of O-ZnO composite nanostructure semiconductor material may further comprise the steps:
(1) preparation Cu
2The O micron particle
Cupric chloride, polyvinylpyrrolidone, salt of wormwood are mixed stirring with Tripotassium Citrate, wait to become blue back and add glucose, in 80 ℃ of vacuum reactions 2 hours, cooling obtained the lobate Cu of four hornbeams by washing, oven dry
2The O micron particle.
(2) preparation ZnO nano particle
Urea soln is mixed stirring with zinc chloride, reacted 6 hours down for 140 ℃ through vacuum, the washing of cooling back obtains the ZnO nano particle.
(3) compound
With the lobate Cu of described four hornbeams
2The O micron particle is dissolved in the deionized water that contains polymine, is heated to 90 ℃ of reactions, and cooling also obtains Cu after washing
2O-PEI solution; Add described ZnO nano particle, obtain Cu through mixing stirring, supersound process
2O-PEI-ZnO precipitation is through washing after, drip to be applied on the silicon chip and in 80 ℃ and dry down; Under argon shield, carry out short annealing, prepare the lobate Cu of four hornbeams
2O-ZnO composite nanostructure semiconductor material.
The lobate Cu of the present invention four hornbeams
2Among the preparation method of O-ZnO composite nanostructure semiconductor material, described mixing is stirred and by magnetic stirrer solution is evenly stirred.The magnetic stirrer that adopts among the preparation method of the present invention, its key part are the stirring magnetons that the base made by annulus and a fritter are made by magnetite.After placing the beaker that solution to be measured is housed on the base, will stir magneton and put into solution, with the logical alternating-current of going up of base, the alternating electromagnetic field that is produced by electromagnetic induction drives the uniform rotation in solution of little magneton, can reach the purpose of even stirred solution.
The lobate Cu of the present invention four hornbeams
2Among the preparation method of O-ZnO composite nanostructure semiconductor material, being reflected in the autoclave of described step (1), (2) carried out, and described autoclave inner tube material is tetrafluoroethylene, and outer tube material is stainless steel.The autoclave that adopts among the preparation method of the present invention, it is overlapped mutually by two root radiuses different cylindrical tubes forms, and inner tube material is tetrafluoroethylene, and length is 70mm, and diameter is 44mm; Outer tube material is stainless steel, and length is 92mm, and diameter is 50mm.Question response solution is poured in the interior pipe, interior pipe is put into outer tube, with the outer seal of tube, can in interior pipe, form the environment of high pressure, sealing.
The present invention adopts the branch step process, prepares Cu respectively with hydrothermal synthesis method earlier
2O micrometer structure and ZnO nanostructure adopt low temperature water-bath and thermal anneal process that the two is combined with each other again and obtain Cu
2The O-ZnO composite nanostructure.Utilize the Cu of this method growth
2The O-ZnO composite nanostructure is at the Cu as matrix
2Compound ZnO nano particle assembles on the basis of O micrometer structure, and it not only has micron-sized Cu
2The O matrix, and surperficial with numerous Nanoparticulate projections at it.
The inventive method has overcome Cu
2These two kinds of materials of O and ZnO are because generally being difficult to of causing of thermolability and lattice mismatch technical difficulty of using hydrothermal method or high-temperature thermal annealing method to be combined with each other, and this complex method can be generalized to various Cu
2O and ZnO are little, in the Application of composite of nanostructure.
The invention has the advantages that (1) adopts hydrothermal method in conjunction with water-bath and thermal anneal process first, successfully synthesizes Cu
2The O-ZnO composite nanostructure; (2) utilize polymine to connect Cu earlier
2O and ZnO remove poly-acetimide middle layer by thermal anneal process again, realize Cu
2The good contact at O-ZnO interface, this method are applicable to various different Cu
2O-ZnO micro nano structure compound is not subjected to the restriction of structure and morphology, can be used for synthetic composite structure with efficient efficiency of light energy utilization; (3) preparation method is simple, and cost is low, and good reproducibility is applied widely, and is large-area growth.
The present invention is used in large-area growth Cu of the present invention on the silicon chip substrate
2The O-ZnO composite structure, its unique heterojunction structure and numerous nano surface projection, the energy band structure of full spectral response, characteristics such as high field enhancement factor can realize its application in solar energy photocatalytic and an emission, therefore have huge scientific research value and wide commercial application prospect.
Description of drawings
Fig. 1 is the lobate Cu of four hornbeams
2The X-ray diffractogram of O-ZnO composite nanostructure;
Fig. 2 is the lobate Cu of four hornbeams
2The SEM photo of O micron particle;
Fig. 3 is the lobate Cu of a large amount of four hornbeams
2The SEM photo of O-ZnO composite nanostructure;
Fig. 4 is the lobate Cu of four hornbeams
2The SEM photo of the magnification of O-ZnO composite nanostructure.
Embodiment
In conjunction with following specific embodiments and the drawings, the present invention is described in further detail.Implement process of the present invention, condition, reagent, experimental technique etc., except the following content of mentioning specially, be universal knowledege and the common practise of this area, the present invention is not particularly limited content.
Embodiment
In the present embodiment, the lobate Cu of four hornbeams
2The step of the concrete preparation of O-ZnO composite nanostructure semiconductor material is as follows:
1, the lobate Cu of preparation four hornbeams
2The O micron particle
A) be that solvent is prepared the solution that Cupric Chloride Solution that 5mL concentration is 0.2mol/L and 5mL contain the 0.2g polyvinylpyrrolidone respectively with the deionized water, they are dissolved in the deionized water of 70mL, stirred 10 minutes with magnetic stirrer.
B) with the deionized water be again solvent to prepare solution of potassium carbonate and the 5mL concentration that 5mL concentration is 1mol/L respectively be the potassium citrate solution of 0.6mol/L, these two parts of solution are successively poured in the solution that the first step obtains, in the process of pouring into, keep stirring.
C) be that solvent preparation 5mL concentration is the glucose solution of 1mol/L in addition with the deionized water, after the solution turned blue in second step, glucose solution poured into, stirred 5 minutes.
D) solution that previous step is obtained is poured in the autoclave of 100mL polytetrafluoroethylliner liner and is sealed, and reactor is put into air dry oven, keeps 2 hours under 80 ℃ temperature.
E) power supply of closing loft drier makes its naturally cooling, and the red-brown precipitation in the reactor is collected, and washes repeatedly several times with deionized water and dehydrated alcohol, the precipitation after washing is collected oven dry just obtain the lobate Cu of four hornbeams
2The O micron particle.
2, preparation ZnO nano particle
A) at first with the deionized water be solvent to prepare urea soln and the 10mL concentration that 10mL concentration is 2mol/L respectively be the liquor zinci chloridi of 0.5mol/L, they are dissolved in the deionized water of 80mL, at room temperature stirred 30 minutes with magnetic stirrer.
B) solution that previous step is obtained is poured in the autoclave of 100mL polytetrafluoroethylliner liner and is sealed, and reactor is put into air dry oven, keeps 6 hours under 140 ℃ temperature.
C) close the loft drier naturally cooling, reaction product is placed whizzer centrifugal (6000rpm), collecting precipitation, with the flushing of deionized water and dehydrated alcohol, and the deionized water solution that will contain the ZnO nano particle places loft drier internal heating to 80 ℃ to remove remaining organic impurity.
D) repeat above-mentioned centrifugal-flushing-heat-processed number all over after just obtain being stored in ZnO nano particle in the deionized water, this solution is kept vibrations, be used for following composite steps after several minutes at once.
3, preparation Cu
2The O-ZnO composite nanostructure
The lobate Cu of four hornbeams that a) will obtain
2The O micron particle is dissolved in the 100mL deionized water, adds polymine (PEI, M
W～25000,2g/L), place water-bath naturally cooling after heating 2 hours under 90 ℃ of temperature, obtain Cu
2O-PEI solution.
B) with Cu
2The O-PEI precipitation is collected and with washed with de-ionized water for several times, is placed the 50mL deionized water, again the ZnO nano particle is added above-mentioned solution, and ultrasonic 2 hours, to obtain Cu
2The O-PEI-ZnO precipitation.
C) precipitation that previous step is obtained collects, and cleans for several times with deionized water and dehydrated alcohol, drips to be applied on the silicon chip that cleans up, and places loft drier under 80 ℃ of temperature dry 3 hours.
D) result product that previous step is obtained places high-temperature annealing furnace heating under argon gas and 1000 ℃ of environment to remove PEI and other organic impurity in 5 minutes.Resultant product is Cu
2The O-ZnO composite nanostructure.
Be illustrated in figure 1 as the lobate Cu of four hornbeams
2The X-ray diffractogram of O-ZnO composite nanostructure.Can see that by figure this composite sample is by the Cu of isometric system
2O and hexagonal system ZnO form, and do not see obvious impurity peaks, and the purity of interpret sample is higher.By these sharp-pointed peaks degree of crystallinity height of sample as can be seen.
Be illustrated in figure 2 as the lobate Cu of four hornbeams
2The SEM photo of O micron particle.Can see Cu
2It is lobate that the O micron particle is four hornbeams, at Cu
2O micron particle centre bit is equipped with tangible depression, grows the angle of the structure of foliated lamellar by the central concave place to mutually perpendicular four direction, has the laminate structure of similar tree leaf vein on the surface at the angle of this bladed structure.Cu
2The length and width of O micron particle are of a size of 1.5～3 μ m.
Be illustrated in figure 3 as the lobate Cu of a large amount of four hornbeams
2The SEM photo of O-ZnO composite nanostructure.Can see Cu
2The O micron particle is the quadrangular outer shape of tool still substantially, but the tree leaf vein shape structure on surface is no longer obvious, and this is because a large amount of ZnO nano particles evenly is compounded in Cu
2Cause on the surface of O micron particle.
Be illustrated in figure 4 as the lobate Cu of four hornbeams
2The SEM photo of the magnification of O-ZnO composite nanostructure.Can see Cu
2The O-ZnO composite nanostructure still is four horn shapes, and a large amount of ZnO nano particles evenly are compounded in Cu
2The surface of O micron particle has covered Cu fully
2The tree leaf vein shape structure on O micron particle surface.The diameter of ZnO nano particle is 20～40nm.
With the lobate Cu of the present invention four hornbeams
2O-ZnO composite nanostructure large area deposition on silicon chip substrate obtains having the semiconductor material that unique heterojunction is constructed, and it has characteristics such as numerous nano surface projectioies, the energy band structure of full spectral response, high field enhancement factor.This semiconductor material is applicable to the application in solar energy photocatalytic and the emission.
Protection content of the present invention is not limited to above embodiment.Under the spirit and scope that do not deviate from inventive concept, variation and advantage that those skilled in the art can expect all are included in the present invention, and are protection domain with the appending claims.
Claims (6)
1. lobate Cu of hornbeam
2O-ZnO composite nanostructure semiconductor material is characterized in that, comprises silicon chip substrate and is grown in the lobate Cu of four hornbeams on the described silicon chip
2The O-ZnO composite nanostructure; Wherein, described Cu
2The O-ZnO composite nanostructure is by Cu
2O micron particle and ZnO nano particle are formed, described Cu
2The O micron particle has four hornbeam foliation structures, and described ZnO nano particle covers described Cu
2O micron particle surface; Wherein, described Cu
2O micron particle central position has depression, grows the angle of the structure of foliated lamellar by described recess to mutually perpendicular four direction, and its surface has the tree leaf vein laminate structure.
2. the lobate Cu of four hornbeams according to claim 1
2O-ZnO composite nanostructure semiconductor material is characterized in that, described Cu
2The O micron particle is of a size of 1.5～3 μ m in the length and width direction, and described ZnO nano particle diameter is 20～40nm.
3. lobate Cu of described four hornbeams of claim 1
2The preparation method of O-ZnO composite nanostructure semiconductor material is characterized in that, utilizes hydrothermal synthesis method synthetic Cu respectively
2O micron particle and ZnO nano particle make described ZnO nano particle be compounded in Cu equably with polymine as aid in material
2On the O micron particle, obtain the lobate Cu of described four hornbeams
2O-ZnO composite nanostructure semiconductor material.
4. as the lobate Cu of four hornbeams as described in the claim 3
2The preparation method of O-ZnO composite nanostructure semiconductor material is characterized in that, may further comprise the steps:
(1) preparation Cu
2The O micron particle
Cupric chloride, polyvinylpyrrolidone, salt of wormwood are mixed stirring with Tripotassium Citrate, wait to become blue back and add glucose, in 80 ℃ of vacuum reactions 2 hours, cooling obtained the lobate Cu of four hornbeams by washing, oven dry
2The O micron particle;
(2) preparation ZnO nano particle
Urea soln is mixed stirring with zinc chloride, reacted 6 hours down for 140 ℃ through vacuum, the washing of cooling back obtains the ZnO nano particle;
(3) compound
With the lobate Cu of described four hornbeams
2The O micron particle is dissolved in the deionized water that contains polymine, is heated to 90 ℃ of reactions, and cooling also obtains Cu after washing
2O-PEI solution; Add described ZnO nano particle, obtain Cu through mixing stirring, supersound process
2O-PEI-ZnO precipitation is through washing after, drip to be applied on the silicon chip and in 80 ℃ and dry down; Under argon shield, carry out short annealing, prepare the lobate Cu2O-ZnO composite nanostructure of four hornbeams semiconductor material.
5. according to the lobate Cu of described four hornbeams of claim 4
2The preparation method of O-ZnO composite nanostructure semiconductor material is characterized in that, described mixing is stirred and by magnetic stirrer solution evenly stirred.
6. according to the lobate Cu of described four hornbeams of claim 4
2The preparation method of O-ZnO composite nanostructure semiconductor material is characterized in that, being reflected in the autoclave of described step (1), (2) carried out, and described autoclave inner tube material is tetrafluoroethylene, and outer tube material is stainless steel.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104327574A (en) * | 2014-09-29 | 2015-02-04 | 中国海洋大学 | Micro/nano Cu2O/ZnO composite material, preparation method and application thereof |
| CN104402052A (en) * | 2014-10-30 | 2015-03-11 | 华东师范大学 | TiO2-quantum-dot-and-MoS2-nanometer-flower-combined heterojunction semiconductor material and preparation method thereof |
| CN106732617A (en) * | 2016-12-05 | 2017-05-31 | 安徽理工大学 | A kind of ZnO/Cu2O hetero-junctions novel photocatalysis materials and preparation method thereof |
| CN107224972A (en) * | 2017-07-26 | 2017-10-03 | 齐齐哈尔大学 | Flower ball-shaped structure ZnO/ZnWO4The synthetic method of photochemical catalyst |
| CN108187756A (en) * | 2018-01-03 | 2018-06-22 | 福建农林大学 | A kind of preparation method of memory-type photocatalytic fiber element microballoon |
| CN109126800A (en) * | 2018-07-20 | 2019-01-04 | 西安交通大学 | A kind of preparation method of cuprous oxide-copper-zine oxide composite photo-catalyst |
| CN109160726A (en) * | 2018-09-27 | 2019-01-08 | 江苏华鸥玻璃有限公司 | A kind of high-performance glass and preparation method thereof |
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| CN104327574A (en) * | 2014-09-29 | 2015-02-04 | 中国海洋大学 | Micro/nano Cu2O/ZnO composite material, preparation method and application thereof |
| CN104402052A (en) * | 2014-10-30 | 2015-03-11 | 华东师范大学 | TiO2-quantum-dot-and-MoS2-nanometer-flower-combined heterojunction semiconductor material and preparation method thereof |
| CN104402052B (en) * | 2014-10-30 | 2016-02-10 | 华东师范大学 | TiO 2quantum dot compound MoS 2nano flower heterojunction semiconductor material and preparation method thereof |
| CN106732617A (en) * | 2016-12-05 | 2017-05-31 | 安徽理工大学 | A kind of ZnO/Cu2O hetero-junctions novel photocatalysis materials and preparation method thereof |
| CN106732617B (en) * | 2016-12-05 | 2019-07-12 | 安徽理工大学 | A kind of ZnO/Cu2O heterojunction photocatalysis material and preparation method thereof |
| CN107224972A (en) * | 2017-07-26 | 2017-10-03 | 齐齐哈尔大学 | Flower ball-shaped structure ZnO/ZnWO4The synthetic method of photochemical catalyst |
| CN108187756A (en) * | 2018-01-03 | 2018-06-22 | 福建农林大学 | A kind of preparation method of memory-type photocatalytic fiber element microballoon |
| CN109126800A (en) * | 2018-07-20 | 2019-01-04 | 西安交通大学 | A kind of preparation method of cuprous oxide-copper-zine oxide composite photo-catalyst |
| CN109160726A (en) * | 2018-09-27 | 2019-01-08 | 江苏华鸥玻璃有限公司 | A kind of high-performance glass and preparation method thereof |
| CN109160726B (en) * | 2018-09-27 | 2019-08-13 | 江苏华鸥玻璃有限公司 | A kind of high-performance glass and preparation method thereof |
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Application publication date: 20130904 |