CN103833065B - A kind of method preparing nano cuprous oxide wire with thermal evaporation techniques - Google Patents
A kind of method preparing nano cuprous oxide wire with thermal evaporation techniques Download PDFInfo
- Publication number
- CN103833065B CN103833065B CN201210480525.0A CN201210480525A CN103833065B CN 103833065 B CN103833065 B CN 103833065B CN 201210480525 A CN201210480525 A CN 201210480525A CN 103833065 B CN103833065 B CN 103833065B
- Authority
- CN
- China
- Prior art keywords
- cuprous oxide
- nano cuprous
- thermal evaporation
- copper sheet
- oxide wire
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The invention belongs to technical field of nanometer material preparation, be specifically related to a kind of method preparing nano cuprous oxide wire with thermal evaporation techniques in conjunction with method of glucose reduction.Concrete implementation method is: repeatedly polished with sand paper by copper sheet, then cleans 30 minutes by iron(ic) chloride washing lotion, after to dry after deionized water rinsing, face up, be placed in retort furnace, be rapidly heated after 350 DEG C, keep 15 minutes.After cooling, the dark-grey black copper sheet obtained is soaked in glucose solution and reduces, treat that the dark-grey black overwhelming majority becomes brick-red, obtain nano cuprous oxide wire.The invention has the advantages that and can prepare a large amount of nano cuprous oxide wires with stabilized baseplate quickly and easily.Compared with conventional fabrication techniques, products obtained therefrom nanoscale is obvious, length-to-diameter ratio is high, do not need that a large amount of chemical agent, productive rate are high, method is simple and easy to promote in building-up process.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, be specifically related to a kind of method preparing nano cuprous oxide wire with thermal evaporation techniques in conjunction with method of glucose reduction.
Background technology
One dimension Red copper oxide (Cu
2o) nano material makes it have extremely wide application prospect at numerous areas such as photoelectronics, biology, medical science because of the physics and chemistry characteristic of its uniqueness.Research in recent years finds, Red copper oxide is a kind of p-type semiconductor material, and energy gap is 2.1eV.Due to quantum size effect, nano cuprous oxide shows peculiar optics, electric property.Nano cuprous oxide can inspire electron-hole pair under visible light illumination, there is larger specific surface area and extremely strong adsorptive power, the right recombination probability of photo-generate electron-hole can be reduced simultaneously, can be used for the fields such as photocatalyst, antifouling paint, solar cell.In recent years, related researcher has done a large amount of scientific effort in control synthesis cuprous nano configuration aspects, adopt multiple method to prepare the cuprous oxide nano particle, nano whisker, nano wire, nanotube, nanometer rod etc. of different-shape, but currently used preparation method also mainly concentrate on traditional wet chemistry method, electrochemical process, solid-phase synthesis, vapour phase oxidation process etc.The nano cuprous oxide wire length-to-diameter ratio that great majority obtain is lower, and pattern difficulty controls, particularly preparation process is complicated, and productive rate is not high, therefore more difficult expansion and popularization.
Thermal evaporation (ThermalEvaporation) be one at relatively high temperatures, make material carburation by evaporation or directly use high-temperature gas to be raw material, the compound required for being generated by oxidizing reaction or the novel method directly making it evaporate to reach hypersaturated state to be condensed into solid-state structure to prepare nano material.Prepare nano material with thermal evaporation and there is the advantages such as productive rate is high, morphology controllable, compound with regular structure, can be widely used in multiple fields such as electronics, optics, catalysis, being with a wide range of applications.In thermal evaporation treating processes, nucleation and growth controls, and is the key of nano materials.The factor affecting nucleation is a lot, comprises the equilibrium constant of substrate, temperature of reaction, reaction gas flow speed, reaction pressure and reaction system and degree of supersaturation etc.Usually, as long as control the cohesion rate of nucleus, the growth of core can just be controlled; And the growth controlling core just can control the size of nano material, pattern, structure and physical property.In nano material preparation process, the factor of impact cohesion is a lot, for metal oxide, can be realized the control to its growth by the concentration and oxygen flow controlling vapor phase metal.
Summary of the invention
The object of the present invention is to provide a kind of convenient and swift, productive rate is high, the technology of preparing of regular appearance, simply controlled nano cuprous oxide wire, to promote the practical further of metal-oxide semiconductor (MOS) nano wire.
The present invention is by adopting following technical scheme to realize foregoing invention object:
(1) cleaning of copper sheet and polishing
Cutting 5 × 5cm size, thickness is the copper sheet of 1.0mm, repeatedly polishes 3 ~ 5 minutes with sand paper, then uses iron(ic) chloride washing lotion (5 grams of iron(ic) chloride, being dissolved in 100 milliliters of mass concentrations is in the hydrochloric acid soln of 3%) clean 30 minutes, then for subsequent use to dry after deionized water rinsing;
(2) thermal evaporation process
Copper sheet after step (1) being processed, faces up, is placed in retort furnace, be rapidly heated to 350 DEG C, and keep 15 minutes.The nanowire array of copper oxide that length-to-diameter ratio is greater than 10 can be formed, be attached to copper sheet surface and form dark-grey black film;
(3) Reduction of Glucose
Be soaked in 50 milliliters of glucose solutions by the dark-grey black copper sheet of gained in step (2), react after 2 hours, the dark-grey black overwhelming majority becomes brick-red, obtains nano cuprous oxide wire.
In step (1) described in the inventive method, sand paper used is 300 ~ 500 order fine sandpapers;
In step (2) described in the inventive method, when being rapidly heated, need control heat-up rate is 15 ~ 50 DEG C/min;
In step (3) described in the inventive method, glucose concentration used is 20 ~ 200g/L;
The invention has the advantages that and can prepare a large amount of nano cuprous oxide wires with stabilized baseplate quickly and easily.Compared with conventional fabrication techniques, method simply, do not need a large amount of chemical agents, productive rate high, be easy to promote.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram of nano cuprous oxide wire;
Fig. 2 is that X-ray energy spectrum carries out the result of elemental analyses to nano cuprous oxide wire surface.
Embodiment
Embodiment 1
Cutting 5 × 5cm size, thickness is the copper sheet of 1.0mm, repeatedly polish 3 ~ 5 minutes with 300 order sand paper, then use iron(ic) chloride washing lotion (5 grams of iron(ic) chloride, being dissolved in 100 milliliters of mass concentrations is in the hydrochloric acid soln of 3%) to clean 30 minutes, then to dry after deionized water rinsing, face up, be placed in retort furnace, controlling temperature rise rate is 15 DEG C/min, after reaching 350 DEG C, keep 15 minutes.After cooling, be soaked in the glucose solution of 50 milliliters of 20g/L by the dark-grey black copper sheet obtained, react after 2 hours, the dark-grey black overwhelming majority becomes brick-red, obtains nano cuprous oxide wire.
Gained nano cuprous oxide wire is analyzed under scanning electronic microscope (S4800, Hitachi, Japan), and result shows that the diameter of gained nano cuprous oxide wire is between 20 ~ 50nm, and length-to-diameter ratio is (see Figure of description 1) more than 70; Through energy dispersion X-ray spectrometry, its atomicity of surface C u: O ratio is about 1.96: 1 (see Figure of description 2), proves that most cupric oxide nano line is reduced to nano cuprous oxide wire.
Embodiment 2
Cutting 5 × 5cm size, thickness is the copper sheet of 1.0mm, repeatedly polishes 3 ~ 5 minutes with 400 order sand paper, 30 minutes are cleaned again by iron(ic) chloride washing lotion, then to dry after deionized water rinsing, face up, be placed in retort furnace, controlling temperature rise rate is 30 DEG C/min, after reaching 350 DEG C, keep 15 minutes, be soaked in the glucose solution of 50 milliliters of 120g/L after cooling, react after 2 hours, obtain nano cuprous oxide wire.
Gained nano cuprous oxide wire diameter is between 30 ~ 50nm, and length-to-diameter ratio is greater than 70; Its atomicity of surface C u: O ratio is about 2.1: 1.
Embodiment 3
Cutting 5 × 5cm size, thickness is the copper sheet of 1.0mm, repeatedly polishes 3 ~ 5 minutes with 400 order sand paper, 30 minutes are cleaned again by iron(ic) chloride washing lotion, then to dry after deionized water rinsing, face up, be placed in retort furnace, controlling temperature rise rate is 50 DEG C/min, after reaching 350 DEG C, keep 15 minutes, be soaked in the glucose solution of 50 milliliters of 50g/L after cooling, react after 2 hours, obtain nano cuprous oxide wire.
Gained nano cuprous oxide wire diameter is between 45 ~ 90nm, and length-to-diameter ratio is greater than 50; Its atomicity of surface C u: O ratio is about 2.24: 1.
Embodiment 4
Cutting 5 × 5cm size, thickness is the copper sheet of 1.0mm, repeatedly polishes 3 ~ 5 minutes with 500 order sand paper, 30 minutes are cleaned again by iron(ic) chloride washing lotion, then to dry after deionized water rinsing, face up, be placed in retort furnace, controlling temperature rise rate is 45 DEG C/min, after reaching 350 DEG C, keep 15 minutes, be soaked in the glucose solution of 50 milliliters of 200g/L after cooling, react after 2 hours, obtain nano cuprous oxide wire.
Gained nano cuprous oxide wire diameter is between 10 ~ 40nm, and length-to-diameter ratio is greater than 100; Its atomicity of surface C u: O ratio is about 1.8: 1.
Claims (4)
1. prepare a method for nano cuprous oxide wire with thermal evaporation techniques, it is characterized in that, the process of preparation comprises:
(1) cleaning of copper sheet and polishing
Cutting 5 × 5cm size, thickness is the copper sheet of 1.0mm, repeatedly polishes 3 ~ 5 minutes, then clean 30 minutes by iron(ic) chloride washing lotion with sand paper, then for subsequent use to dry after deionized water rinsing;
(2) thermal evaporation process
Copper sheet after step (1) being processed, faces up, is placed in retort furnace, be rapidly heated to 350 DEG C, and keep 15 minutes, can form the nanowire array of copper oxide that length-to-diameter ratio is greater than 10, is attached to copper sheet surface and forms dark-grey black film;
(3) Reduction of Glucose
Be soaked in 50 milliliters of glucose solutions by the dark-grey black copper sheet of gained in step (2), react after 2 hours, the dark-grey black overwhelming majority becomes brick-red, obtains nano cuprous oxide wire.
2. a kind of method preparing nano cuprous oxide wire with thermal evaporation techniques as described in claim 1, it is characterized in that, in the process (1) of preparation, sand paper used is 300 ~ 500 order fine sandpapers.
3. a kind of method preparing nano cuprous oxide wire with thermal evaporation techniques as described in claim 1, it is characterized in that, in the process (2) of preparation, when being rapidly heated, need control heat-up rate is 15 ~ 50 DEG C/min.
4. a kind of method preparing nano cuprous oxide wire with thermal evaporation techniques as described in claim 1, it is characterized in that, in the process (3) of preparation, glucose concentration used is 20 ~ 200g/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210480525.0A CN103833065B (en) | 2012-11-23 | 2012-11-23 | A kind of method preparing nano cuprous oxide wire with thermal evaporation techniques |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210480525.0A CN103833065B (en) | 2012-11-23 | 2012-11-23 | A kind of method preparing nano cuprous oxide wire with thermal evaporation techniques |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103833065A CN103833065A (en) | 2014-06-04 |
| CN103833065B true CN103833065B (en) | 2015-11-25 |
Family
ID=50797012
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210480525.0A Expired - Fee Related CN103833065B (en) | 2012-11-23 | 2012-11-23 | A kind of method preparing nano cuprous oxide wire with thermal evaporation techniques |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103833065B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106207090B (en) * | 2016-07-29 | 2019-02-15 | 四川大学 | Three-D nano-porous copper/one-dimensional nano cuprous oxide wire network-type negative electrode of lithium ion battery and one one-step preparation method |
| CN108504984A (en) * | 2018-04-27 | 2018-09-07 | 厦门大学 | A kind of super-hydrophobic composite construction preparation method of cupric oxide nano line |
| CN109748314A (en) * | 2019-03-25 | 2019-05-14 | 郑州大学 | A kind of preparation method of no template nano cuprous oxide wire array |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102051675A (en) * | 2010-10-28 | 2011-05-11 | 中山大学 | Method for manufacturing CuO nanowire |
| CN102104077A (en) * | 2010-10-28 | 2011-06-22 | 中山大学 | Manufacturing method for nanowire with CuO/ZnO core/shell structure |
| CN102776469A (en) * | 2012-07-27 | 2012-11-14 | 中山大学 | Method for preparing copper nanowires and copper nano pointed cones |
-
2012
- 2012-11-23 CN CN201210480525.0A patent/CN103833065B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102051675A (en) * | 2010-10-28 | 2011-05-11 | 中山大学 | Method for manufacturing CuO nanowire |
| CN102104077A (en) * | 2010-10-28 | 2011-06-22 | 中山大学 | Manufacturing method for nanowire with CuO/ZnO core/shell structure |
| CN102776469A (en) * | 2012-07-27 | 2012-11-14 | 中山大学 | Method for preparing copper nanowires and copper nano pointed cones |
Non-Patent Citations (2)
| Title |
|---|
| "Polyhedral 50-Facet Cu2O Microcrystals Partially Enclosed by {311} High-Index Planes: Synthesis and Enhanced Catalytic CO Oxidation Activity";Mei Leng et al.;《J. Am. Chem. Soc.》;20101112;第132卷(第48期);第17084–17087页 * |
| 严新等."氧化铜和氧化亚铜".《无机及分析化学》.北京大学出版社,2011,(第1版),第310页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103833065A (en) | 2014-06-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zeng et al. | Fabrication of pn heterostructure ZnO/Si moth-eye structures: Antireflection, enhanced charge separation and photocatalytic properties | |
| Wang et al. | Ferroelectric BaTiO3@ ZnO heterostructure nanofibers with enhanced pyroelectrically-driven-catalysis | |
| Jiao et al. | Synthesis of Z-scheme g-C3N4/PPy/Bi2WO6 composite with enhanced visible-light photocatalytic performance | |
| Rani et al. | Sn doped α-Fe2O3 (Sn= 0, 10, 20, 30 wt%) photoanodes for photoelectrochemical water splitting applications | |
| CN104538597B (en) | Preparation method of snowflake titanium dioxide/two-dimensional nanometre titanium carbide composite material | |
| Saravanan et al. | Growth and characterization of spray pyrolysis deposited copper oxide thin films: Influence of substrate and annealing temperatures | |
| CN105329876B (en) | A kind of preparation method of boron, nitrogen co-doped carbon quantum dot | |
| CN101372330B (en) | Method for coating carbon nano-tube with metal doped zinc oxide nano-particle | |
| CN105363483A (en) | Preparation method of titanium dioxide nanowire/two-dimensional layered titanium carbide composite material | |
| CN101412505A (en) | Preparation of high-purity tin diselenide nano-plate | |
| CN103252228A (en) | Preparation method of composite nanomaterial of nano ZnO and graphene nanosheet | |
| CN110586931B (en) | Ultra-long silver nanowire and preparation method thereof | |
| CN102275908A (en) | Preparation method of graphene material | |
| CN104874811A (en) | Preparing method of simple substance bismuth/bismuth compound nanocomposite with oxygen vacancies | |
| CN103908969A (en) | Preparation method of BiFeO3 nano particle compounded TiO2 nanotube array electrode material | |
| CN101724839B (en) | Micron/nanoscale BiOCl film material and preparation method thereof | |
| CN103833065B (en) | A kind of method preparing nano cuprous oxide wire with thermal evaporation techniques | |
| Su et al. | Electrochemically assisted photocatalytic degradation of phenol using silicon-doped TiO2 nanofilm electrode | |
| CN103626163A (en) | Graphene preparation method | |
| Pirgholi-Givi et al. | The influence of preparation parameters on the photocatalytic performance of mixed bismuth titanate-based nanostructures | |
| Jia et al. | Achieving excellent photocatalytic degradation of pollutants by flower-like SrBi4Ti4O15/BiOCl heterojunction: The promotion of piezoelectric effect | |
| CN105562040A (en) | Preparation and application of BiOCl-(001)/GO nano-composite photocatalyst | |
| Wang et al. | Synergetic piezo-photocatalytic effect in SbSI for highly efficient degradation of methyl orange | |
| CN106238077B (en) | A kind of carbon fiber@molybdenum disulfide nano sheet core-shell structure and preparation method thereof | |
| CN104692387B (en) | A kind of method using silicon containing biomass as raw material low temperature preparation nanometer silicon carbide and preparation-obtained nanometer silicon carbide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20151125 Termination date: 20181123 |