CN103833065A - Method for preparing cuprous oxide nanowire by thermal evaporation technique - Google Patents
Method for preparing cuprous oxide nanowire by thermal evaporation technique Download PDFInfo
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- CN103833065A CN103833065A CN201210480525.0A CN201210480525A CN103833065A CN 103833065 A CN103833065 A CN 103833065A CN 201210480525 A CN201210480525 A CN 201210480525A CN 103833065 A CN103833065 A CN 103833065A
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Abstract
The invention belongs to the technical field of nano material preparation, and in particular to a method for preparing cuprous oxide nanowire by thermal evaporation technique combined with a glucose reduction method. The specific implementation method is as below: repeatedly polishing the copper sheet with sandpaper, washing with ferric chloride solution for 30 min, washing with deionized water, carrying out air-drying, placing the copper sheet with the right face upwards in a muffle furnace, fast heating to 350 DEG C, and keeping for 15 min; and after cooling, immersing obtained dark grey black copper sheet in a glucose solution for reduction, and acquiring cuprous oxide nano wire when most of the grey black turns to brick red. The invention has the advantage that the method can easily and quickly prepare a lot of cuprous oxide nanowires with stable bases. Compared with the traditional preparation technology, the obtained product has obviously nano scale and high draw ratio; and the synthetic process does not need a large number of chemicals, reaches high yield, and is simple and easy to popularize.
Description
Technical field
The invention belongs to nano material preparing technical field, be specifically related to a kind of method of 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 its unique physics and chemistry characteristic.Research discovery in recent years, Red copper oxide is a kind of p-type semiconductor material, 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 radiation of visible light, there is larger specific surface area and extremely strong adsorptive power, can reduce the right recombination probability in light induced electron-hole, can be used for the fields such as photocatalyst, antifouling paint, solar cell simultaneously.In recent years, related researcher has done a large amount of scientific efforts in the synthetic cuprous nano structure aspects of control, adopt several different methods to prepare the cuprous oxide nano particle of different-shape, nano whisker, nano wire, nanotube, nanometer rod etc., 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, pattern difficult control, particularly preparation process complexity, and productive rate is not high, therefore more difficult expansion and popularization.
Thermal evaporation (Thermal Evaporation) is a kind of under comparatively high temps, make material carburation by evaporation or directly use high-temperature gas for raw material, generate needed compound or directly make its evaporation reach hypersaturated state by oxidizing reaction and be condensed into the novel method that solid-state structure is prepared nano material.Prepare nano material with thermal evaporation and there is the advantages such as productive rate is high, pattern is controlled, compound with regular structure, can be widely used in multiple fields such as electronics, optics, catalysis, be with a wide range of applications.In thermal evaporation treating processes, nucleation and growth control, is the key of nano materials.The factor that affects nucleation is a lot, comprises the equilibrium constant and the degree of supersaturation etc. of substrate, temperature of reaction, reaction gas flow speed, reaction pressure and reaction system.Usually, as long as control the cohesion rate of nucleus, just can control the growth of core; And the growth of controlling core just can be controlled size, pattern, structure and the physical property of nano material.In nano material preparation process, the factor of impact cohesion is a lot, for metal oxide, can realize the control to its growth by concentration and the oxygen flow of 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, pattern is regular, the technology of preparing of simple controlled nano cuprous oxide wire, to promote the further practical 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, then use iron(ic) chloride washing lotion (5 grams of iron(ic) chloride with sand paper, be dissolved in the hydrochloric acid soln that 100 milliliters of mass concentrations are 3%) clean 30 minutes, then for subsequent use to dry after deionized water rinsing;
(2) thermal evaporation processing
By step (1) copper sheet after treatment, face up, be 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, be attached to copper sheet surface and form dark-grey black film;
(3) Reduction of Glucose
The dark-grey black copper sheet of gained in step (2) is soaked in 50 milliliters of glucose solutions, reacts after 2 hours, the dark-grey black overwhelming majority becomes brick-red, obtains nano cuprous oxide wire.
In step described in the inventive method (1), sand paper used is 300～500 order fine sandpapers;
In step described in the inventive method (2), while being rapidly heated, needing to control heat-up rate is 15～50 DEG C/min;
In step described in the inventive method (3), glucose solution concentration used is 20～200g/L;
The invention has the advantages that and can prepare quickly and easily a large amount of nano cuprous oxide wires with stabilized baseplate.Compared with traditional technology of preparing, method simply, do not need a large amount of chemical agents, productive rate high, be easy to promote.
Brief description of the drawings
Fig. 1 is the scanning electron microscope diagram of nano cuprous oxide wire;
Fig. 2 is X-ray energy spectrum carries out ultimate analysis qualification result 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, are dissolved in the hydrochloric acid soln that 100 milliliters of mass concentrations are 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, reach after 350 DEG C, keep 15 minutes.After cooling, the dark-grey black copper sheet obtaining is soaked in the glucose solution of 50 milliliters of 20g/L, to 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 exceedes 70 (seeing Figure of description 1); Through the spectrometry of energy dispersion X ray, the atomicity ratio of its surface C u: O is about 1.96: 1 (seeing Figure of description 2), proves that most cupric oxide nano line has been reduced to nano cuprous oxide wire.
Embodiment 2
Cutting 5 × 5cm size, the copper sheet that thickness is 1.0mm, polishes 3～5 minutes repeatedly with 400 order sand paper, clean 30 minutes by iron(ic) chloride washing lotion again, then, to dry after deionized water rinsing, face up, be placed in retort furnace, controlling temperature rise rate is 30 DEG C/min, reach after 350 DEG C, keep 15 minutes, after cooling, be soaked in the glucose solution of 50 milliliters of 120g/L, 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; The atomicity ratio of its surface C u: O is about 2.1: 1.
Embodiment 3
Cutting 5 × 5cm size, the copper sheet that thickness is 1.0mm, polishes 3～5 minutes repeatedly with 400 order sand paper, clean 30 minutes by iron(ic) chloride washing lotion again, then, to dry after deionized water rinsing, face up, be placed in retort furnace, controlling temperature rise rate is 50 DEG C/min, reach after 350 DEG C, keep 15 minutes, after cooling, be soaked in the glucose solution of 50 milliliters of 50g/L, 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; The atomicity ratio of its surface C u: O is about 2.24: 1.
Embodiment 4
Cutting 5 × 5cm size, the copper sheet that thickness is 1.0mm, polishes 3～5 minutes repeatedly with 500 order sand paper, clean 30 minutes by iron(ic) chloride washing lotion again, then, to dry after deionized water rinsing, face up, be placed in retort furnace, controlling temperature rise rate is 45 DEG C/min, reach after 350 DEG C, keep 15 minutes, after cooling, be soaked in the glucose solution of 50 milliliters of 200g/L, 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; The atomicity ratio of its surface C u: O is about 1.8: 1.
Claims (4)
1. a method of preparing nano cuprous oxide wire with thermal evaporation techniques, 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 use iron(ic) chloride washing lotion (5 grams of iron(ic) chloride with sand paper, be dissolved in the hydrochloric acid soln that 100 milliliters of mass concentrations are 3%) clean 30 minutes, then for subsequent use to dry after deionized water rinsing;
(2) thermal evaporation processing
By step (1) copper sheet after treatment, face up, be 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, be attached to copper sheet surface and form dark-grey black film;
(3) Reduction of Glucose
The dark-grey black copper sheet of gained in step (2) is soaked in 50 milliliters of glucose solutions, reacts after 2 hours, the dark-grey black overwhelming majority becomes brick-red, obtains nano cuprous oxide wire.
2. as described in claim 1 in synthesis step (1), sand paper used is 300～500 order fine sandpapers.
3. as described in claim 1 in synthesis step (2), while being rapidly heated, needing to control heat-up rate be 15～50 DEG C/min.
4. as described in claim 1 in synthesis step (3), glucose solution concentration used is 20～200g/L.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106207090A (en) * | 2016-07-29 | 2016-12-07 | 四川大学 | Three-D nano-porous copper/one-dimensional nano cuprous oxide wire network-type lithium ion battery negative 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 |
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| 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 |
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2012
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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 |
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| MEI LENG ET AL.: ""Polyhedral 50-Facet Cu2O Microcrystals Partially Enclosed by {311} High-Index Planes: Synthesis and Enhanced Catalytic CO Oxidation Activity"", 《J. AM. CHEM. SOC.》 * |
| 严新等: "《无机及分析化学》", 30 September 2011, 北京大学出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106207090A (en) * | 2016-07-29 | 2016-12-07 | 四川大学 | Three-D nano-porous copper/one-dimensional nano cuprous oxide wire network-type lithium ion battery negative and one one-step preparation method |
| 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 |
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