CN104445359B - A kind of method preparing cuprous nano structure on phosphor bronze surface - Google Patents
A kind of method preparing cuprous nano structure on phosphor bronze surface Download PDFInfo
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- CN104445359B CN104445359B CN201410651195.6A CN201410651195A CN104445359B CN 104445359 B CN104445359 B CN 104445359B CN 201410651195 A CN201410651195 A CN 201410651195A CN 104445359 B CN104445359 B CN 104445359B
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Abstract
The invention belongs to the preparing technical field of Red copper oxide, particularly disclose a kind of method preparing cuprous nano structure on phosphor bronze surface.Comprise the following steps: the phosphor bronze base material after cleaning is immersed in water by (1), and temperature control reacts 1 ~ 24h at 5 ~ 60 DEG C of temperature; (2) reacted for step (1) phosphor bronze base material is dried up through nitrogen, after drying, obtain cuprous nano structure.Present method is a kind of simple preparation method, time saving and energy saving, does not need extra main equipment, does not need extra operation; The whole preparation process of present method is all carried out in water, and do not use other any reagent, preparation cost is low; Present method environmental friendliness, can not environmental danger to external world.
Description
Technical field
The invention belongs to the preparing technical field of Red copper oxide, particularly a kind of method preparing cuprous nano structure on phosphor bronze surface.
Background technology
Red copper oxide is a kind of p-N-type semiconductorN, and due to its rich reserves, nontoxic, preparation cost is low, has potential application in a lot of field.Such as grade cuprous oxide is at photoelectric device (R.N.Briskman, AStudyofElectrodepositedCuprousOxidePhotovoltaicCells.So l.EnergyMater.Sol.Cells1992,27,361 366.), catalysis (P.E.Jongh, D.Vanmaelkelbergh, J.J.Kelly, Cu
2o:aCatalystforthePhotochemicalDecompositionofWater Chem.Commun.1999,12,1,069 1074.), lithium ion battery (B.White, M.Yin, A.Hall, D.Le, N.Turro, CompleteCOOxidationoverCu
2oNanoparticlesSupportedonSilicaGel.NanoLett.2006,6,2,095 2102.) etc. field is widely used.Usually the method preparing grade cuprous oxide has thermal oxidation method (H.H.Lee, C.Lee, Y.L.Kuo, Y.W.Yen, ANovelTwo-StepMOCVDforProducingThinCopperFlmswithaMixtur eofEthylAlcoholandWaterastheAdditive.ThinSolidFilms2006, 498, 43 52.), chemical Vapor deposition process (L.S.Huang, S.G.Yang, T.Li, Y.W.Du, Y.N.Lu, S.Z.Shi, PreparationofLarge-ScaleCupricOxideNanowiresbyThermalEva porationMethod.J.Cryst.Growth2004, 260, 130 137.), electrochemical deposition method (Y.B.Ding, Y.Li, L.L.Yang, Z.Y.Li, W.H.Xin, X.Liu, L.Pan, J.P.Zhao, TheFabricationofControlledCoral-likeCu
2oFilmsandTheirHydrophobicProperty.Appl.Surf.Sci.2009,131,2,561 2569.) etc.But there are some shortcomings more or less in these methods.High-temperature technology as: thermal oxidation method can cause oxygen to spread and lattice dilatation and cause that dislocation lacks, lattice distortion even pyrolytic decomposition, in increase photoelectric conversion process current carrier compound probability and reduce solar battery efficiency.Chemical Vapor deposition process needs main equipment, complicated operation, needs strict control, be unfavorable for scale operation for all kinds of parameters in deposition process.The method of electrochemical deposition is the relatively simple method of one, major advantage has that equipment is simple, easy to operate, reaction conditions is gentle, be suitable for the advantages such as large-scale commercial production, but this method also affects by several factors, as: current density, organic additive, pH value, temperature etc., exacting terms also can affect its further commercial applications.Although above preparation method can prepare excellent grade cuprous oxide, these methods often also also exist consuming time, effort, with high costs, need main equipment, severe reaction conditions, more responsive to temperature, pressure, the shortcomings such as environment is unfriendly.Therefore, simple, low cost, eco-friendly preparation method still very Worth Expecting.
Summary of the invention
The object of the present invention is to provide a kind of method preparing cuprous nano structure on phosphor bronze surface, the method is simple, low cost, environmental friendliness.
For achieving the above object, the technical scheme taked of the present invention is as follows:
Prepare a method for cuprous nano structure on phosphor bronze surface, comprise the following steps:
(1) be immersed in water by the phosphor bronze base material after cleaning, temperature control reacts 1 ~ 24h at 5 ~ 60 DEG C of temperature;
(2) reacted for step (1) phosphor bronze base material is dried up through nitrogen, after drying, obtain cuprous nano structure.
In step (1), acetone (organism of removing phosphor bronze substrate surface) is first used to use dust technology (oxide compound of removing phosphor bronze substrate surface) to clean phosphor bronze base material afterwards.
In step (2), the reacted phosphor bronze base material of step (1) first dries up through nitrogen with after water cleaning (impurity unavoidably fallen in removing reaction process) again.
Further, described phosphor bronze base material is phosphor bronze sheet or phosphor bronze netting.
Further, described phosphor bronze base material is the phosphor bronze sheet or the phosphor bronze netting that meet alloy designations C5111, C5101, C5191, C5212, C5210.
Further, described water is for meeting the one-level water of water for analytical laboratory use standard GB/T/T6682-2008, secondary water or tertiary effluent, or the distilled water for preparing by the method for one or many distillation.
Preferably, preferred temperature control reacts 3 ~ 5h at 15 ~ 45 DEG C of temperature.
Further, the shape of described cuprous nano structure is particulate state, bar-shaped or block, and its size is between 10 ~ 800nm.
Compared with prior art, the beneficial effect had is in the present invention:
(1) present method is a kind of simple preparation method, time saving and energy saving, does not need extra main equipment, does not need extra operation.
(2) the whole preparation process of present method is all carried out in water, and do not use other any reagent, preparation cost is low.
(3) present method environmental friendliness, can not environmental danger to external world.
Accompanying drawing explanation
Fig. 1 is the SEM photo of the cuprous nano structure that embodiment 1 obtains.
Fig. 2 is the SEM photo of the cuprous nano structure that embodiment 2 obtains.
Fig. 3 is the XRD figure spectrum of the cuprous nano structure that embodiment 2 obtains.
Fig. 4 is the SEM photo of the cuprous nano structure that embodiment 3 obtains.
Fig. 5 is the SEM photo of the cuprous nano structure that embodiment 4 obtains.
Fig. 6 is the SEM photo of the cuprous nano structure that embodiment 5 obtains.
Fig. 7 is the SEM photo of the cuprous nano structure that embodiment 6 obtains.
Embodiment
Embodiment 1: be immersed in the middle of water after the cleaning of the nitric acid of acetone and 0.1M successively by the phosphor bronze netting of trade mark C5212, temperature of reaction is room temperature (15 DEG C), and the reaction times is 3 hours, after reaction terminates, phosphor bronze netting water is cleaned 3 times, and nitrogen dries up, and is drying to obtain sample; The water adopted in the present embodiment is for meeting the one-level water of water for analytical laboratory use standard GB/T/T6682-2008.As shown in Figure 1, measuring the cuprous nanostructure of this sample oxidation through SEM is that the particle packing of about 60 ~ 110nm forms.
Embodiment 2: be immersed in the middle of water by the phosphor bronze netting of trade mark C5212 after the nitric acid cleaning of acetone and 0.1M, temperature of reaction is room temperature (25 DEG C), and the reaction times is 3 hours, after reaction terminates, phosphor bronze netting water is cleaned 3 times, and nitrogen dries up, and is drying to obtain sample; The water adopted in the present embodiment is for meeting the secondary water of water for analytical laboratory use standard GB/T/T6682-2008.As shown in Figure 2, the cuprous nano structure measuring this sample through SEM is the club shaped structure of about 90 ~ 110nm, and club shaped structure becomes 90 degree of growths of reporting to the leadship after accomplishing a task.Fig. 3 is the XRD figure spectrum of sample, as seen from the figure: the strong peak of black dot mark represents cubic copper phase in phosphor bronze netting (JCPDS card No.77-3038), the small peak of black diamonds mark is highly consistent with Red copper oxide crystalline phase (JCPDS card No.65-3288), demonstrates phosphor bronze netting surface and there is cuprous oxide crystal.
Embodiment 3: be immersed in the middle of water by the phosphor bronze netting of trade mark C5212 after the nitric acid cleaning of acetone and 0.1M, temperature of reaction is room temperature (35 DEG C), and the reaction times is 3 hours, after reaction terminates, phosphor bronze netting water is cleaned 3 times, and nitrogen dries up, and is drying to obtain sample; The water adopted in the present embodiment is for meeting the tertiary effluent of water for analytical laboratory use standard GB/T/T6682-2008.As shown in Figure 4, the cuprous nano structure measuring this sample through SEM comprises large lumphy structure, grainy texture and club shaped structure (size is between 40 ~ 400nm).
Embodiment 4: be immersed in the middle of water by the phosphor bronze netting of trade mark C5212 after the nitric acid cleaning of acetone and 0.1M, temperature of reaction is room temperature (45 DEG C), and the reaction times is 3 hours, after reaction terminates, phosphor bronze netting water is cleaned 3 times, and nitrogen dries up, and is drying to obtain sample; The water adopted in the present embodiment is first water.As shown in Figure 5, the cuprous nano structure measuring this sample through SEM is mainly lumphy structure, and grainy texture (between size 40 ~ 800nm) is arranged at bottom.
Embodiment 5: be immersed in the middle of water by the phosphor bronze sheet of trade mark C5210 after the nitric acid cleaning of acetone and 0.1M, temperature of reaction is room temperature (35 DEG C), and the reaction times is 5 hours, after reaction terminates, phosphor bronze sheet water is cleaned 3 times, and nitrogen dries up, and is drying to obtain sample; The water adopted in the present embodiment is redistilled water.As shown in Figure 6, the cuprous nano structure measuring this sample through SEM is the bar-shaped or lumphy structure that stratiform is piled up, and club shaped structure surface is projection (size is between 60 ~ 800) particularly.
Embodiment 6: be immersed in the middle of water by the phosphor bronze sheet of trade mark C5210 after the nitric acid cleaning of acetone and 0.1M, temperature of reaction is room temperature (25 DEG C), and the reaction times is 3 hours, after reaction terminates, phosphor bronze sheet water is cleaned 3 times, and nitrogen dries up, and is drying to obtain sample; The water adopted in the present embodiment is three distilled water.As shown in Figure 7, the cuprous nano structure measuring this sample through SEM is the nano bar-shape structure of particle packing, structure comparison regular (between size 60-500 nanometer).
Claims (7)
1. prepare a method for cuprous nano structure on phosphor bronze surface, it is characterized in that comprising the following steps:
(1) be immersed in water by the phosphor bronze base material after cleaning, temperature control reacts 1 ~ 24h at 5 ~ 60 DEG C of temperature;
(2) reacted for step (1) phosphor bronze base material is dried up through nitrogen, after drying, obtain cuprous nano structure.
2. method according to claim 1, is characterized in that: in step (1), first cleans phosphor bronze base material with after acetone with dust technology.
3. method according to claim 1, is characterized in that: in step (2), is first dried up through nitrogen with after water cleaning by reacted for step (1) phosphor bronze base material again.
4., according to the arbitrary described method of claim 1-3, it is characterized in that: described phosphor bronze base material is phosphor bronze sheet or phosphor bronze netting.
5. method according to claim 4, is characterized in that: described phosphor bronze base material is the phosphor bronze sheet or the phosphor bronze netting that meet alloy designations C5111, C5101, C5191, C5212, C5210.
6. according to the arbitrary described method of claim 1-3, it is characterized in that: described water is for meeting the one-level water of water for analytical laboratory use standard GB/T/T6682-2008, secondary water or tertiary effluent, or the distilled water for preparing by the method for one or many distillation.
7., according to the arbitrary described method of claim 1-3, it is characterized in that: temperature control reacts 3 ~ 5h at 15 ~ 45 DEG C of temperature.
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| CN102618925A (en) * | 2012-04-13 | 2012-08-01 | 青岛大学 | Preparation method of cuprous oxide (CU2O) nano octahedral materials |
| CN103112883A (en) * | 2012-12-10 | 2013-05-22 | 浙江理工大学 | Method for preparing superfine cuprous oxide powder |
| CN103172104A (en) * | 2013-04-03 | 2013-06-26 | 浙江理工大学 | Preparation method of nano cuprous oxide |
| CN103787402A (en) * | 2014-01-23 | 2014-05-14 | 复旦大学 | Method for preparing cuprous oxide nanowire material |
| CN103787401A (en) * | 2014-01-16 | 2014-05-14 | 复旦大学 | Cuprous oxide nanowire material and preparation method thereof |
| CN104030338A (en) * | 2013-04-03 | 2014-09-10 | 浙江理工大学 | Preparation method of hollow cubic cuprous oxide nano material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP2791059A1 (en) * | 2013-01-14 | 2014-10-22 | Kaya, Cengiz | A method for production and coating of antibacterial copper (ii) oxide (cuo) nano-tube |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618925A (en) * | 2012-04-13 | 2012-08-01 | 青岛大学 | Preparation method of cuprous oxide (CU2O) nano octahedral materials |
| CN103112883A (en) * | 2012-12-10 | 2013-05-22 | 浙江理工大学 | Method for preparing superfine cuprous oxide powder |
| CN103172104A (en) * | 2013-04-03 | 2013-06-26 | 浙江理工大学 | Preparation method of nano cuprous oxide |
| CN104030338A (en) * | 2013-04-03 | 2014-09-10 | 浙江理工大学 | Preparation method of hollow cubic cuprous oxide nano material |
| CN103787401A (en) * | 2014-01-16 | 2014-05-14 | 复旦大学 | Cuprous oxide nanowire material and preparation method thereof |
| CN103787402A (en) * | 2014-01-23 | 2014-05-14 | 复旦大学 | Method for preparing cuprous oxide nanowire material |
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