CN108504984A - A kind of super-hydrophobic composite construction preparation method of cupric oxide nano line - Google Patents
A kind of super-hydrophobic composite construction preparation method of cupric oxide nano line Download PDFInfo
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- CN108504984A CN108504984A CN201810391335.9A CN201810391335A CN108504984A CN 108504984 A CN108504984 A CN 108504984A CN 201810391335 A CN201810391335 A CN 201810391335A CN 108504984 A CN108504984 A CN 108504984A
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- copper sheet
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/10—Oxidising
- C23C8/12—Oxidising using elemental oxygen or ozone
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/02—Pretreatment of the material to be coated
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Abstract
A kind of super-hydrophobic composite construction preparation method of cupric oxide nano line, is related to nano material.Cleaning treatment is carried out to copper sheet surface；Surface Texture is carried out to copper sheet using laser, micro-structure is formed on copper sheet surface；Cleaning treatment is carried out to the copper sheet after Surface Texture；It is cooled to room temperature by the copper sheet heating after cleaning treatment, then by copper sheet, micro-nano compound structure cupric oxide nano line is obtained on copper sheet surface；Micro-nano compound structure cupric oxide nano line is modified using low-surface-energy material, the super hydrophobic surface of cupric oxide nano line micro-nano compound structure is obtained after drying.Obtained cupric oxide nano line micro-nano compound structure surface has super-hydrophobicity, and cupric oxide nano line durability is stronger, is not easily broken or peels off, and can be widely applied to the fields such as biosensing device, novel photoelectric-detection.
Description
Technical field
The present invention relates to nano materials, more particularly, to a kind of super-hydrophobic composite construction preparation side of cupric oxide nano line
Method.
Background technology
Super hydrophobic surface refers generally to be more than 150 ° with water contact angle, and roll angle is less than 10 ° of surface (the gloomy of Su Fenghua, Liu Can
Aluminium material surface based superhydrophobic thin films and preparation method thereof:,CN104131322A[P].2014).Super hydrophobic surface has " lotus leaf because of it
Effect " has huge application potential in anticorrosion, self-cleaning surface etc..Currently, the method for construction super hydrophobic surface can
It is divided into two kinds：One is modified using low-surface energy substance in solid substrate surface；Another kind is to solid substrate table
Face carries out texture texture.
Metal oxide is n-type semiconductor mostly, and copper oxide is one of p-type semiconductor material few in number (Du Zu
Bright, Qiao Zhencong, Cheng Ke wait a kind of preparation methods of nanowire array of copper oxide film of:,CN102181831A[P].2011).
Cupric oxide nano tape gap has good catalytic property and the absorption coefficient of light between 1.2~1.9eV, is a kind of fine
Gas and humidity sensor material.Compared to traditional bulk material, one-dimensional cupric oxide nano wire material is due to small size
Effect has more superior performance in field of nanometer technology, has been to be concerned by more and more people and study.
Currently, the synthetic method of one-dimensional cupric oxide nano line has hydro-thermal method, thermal oxidation method, template and anodizing
Deng, but respectively have its limitation.Wherein thermal oxidation method, i.e., using copper as substrate, by controlling suitable temperature and time, in air or
It is aoxidized under oxygen atmosphere, prepares the cupric oxide nano line of vertical substrate, be that a kind of cost is minimum, oxidation process is most simple
It is single, the convenient method prepared on a large scale.But cupric oxide nano line film and substrate binding force prepared by this method is very weak, be easy from
It cracks or peels off on substrate, limit the application of cupric oxide nano line in practice；In addition the copper oxide that prepared by thermal oxidation method is received
Rice noodles do not have super-hydrophobicity, and durability, anticorrosive property and self-cleaning surface ability are also poor, have to practical application certain
Limitation.
Invention content
The purpose of the present invention is to provide can overcome cupric oxide nano line film durability prepared by current thermal oxidation method it is poor,
A kind of super-hydrophobic composite construction preparation method of the cupric oxide nano line for the defects of being easy cracking or peeling off.
The present invention includes the following steps：
1) cleaning treatment is carried out to copper sheet surface；
2) Surface Texture is carried out to copper sheet using laser, micro-structure is formed on copper sheet surface；
3) cleaning treatment is carried out to the copper sheet after step 2) Surface Texture；
4) copper sheet after cleaning treatment is heated, then copper sheet is cooled to room temperature, micro-nano composite junction is obtained on copper sheet surface
Structure cupric oxide nano line；
5) micro-nano compound structure cupric oxide nano line is modified using low-surface-energy material, is aoxidized after drying
The super hydrophobic surface of copper nano-wire micro-nano compound structure.
In step 1), the specific method that cleaning treatment is carried out to copper sheet surface can be：Copper sheet sample is positioned over
It fills and is cleaned in the ultrasonic washing instrument of deionized water, the copper sheet sample cleaned up is put into after being impregnated in dilute hydrochloric acid and is taken
Go out, then with washes of absolute alcohol, compressed nitrogen is used in combination to dry up, obtains clean copper sheet sample.
It is described that Surface Texture is carried out to copper sheet using laser in step 2), form the specific of micro-structure on copper sheet surface
Method can be：Using laser surface texture technology, regulate after optical fiber laser related processing parameters to clean copper sheet surface into
Row laser scanning is handled, and special two-dimensional structure is processed on copper sheet surface, realizes controllable array micrometer structure.
In step 3), the specific method that the copper sheet after the Surface Texture to step 2) carries out cleaning treatment can be：It will
Copper sheet after step 2) Surface Texture is cleaned by ultrasonic in ethyl alcohol, is dried up with compressed nitrogen after then being rinsed with deionized water.
It is described using thermal oxidation method growth oxidation copper nano-wire in step 4), it is multiple to provide a micro-nano on copper sheet surface
Close structure；Using the special two-dimensional structure in copper sheet surface as substrate, reduces the thermal stress of cupric oxide nano line film, make cupric oxide nano
Line film is not easily susceptible to cracking or peels off；The heating can carry out open heating on hot plate, and the temperature of heating can be 300~
600 DEG C, the time of heating can be 3~5h.
The cupric oxide nano line micro-nano compound structure surface that the present invention obtains has super-hydrophobicity, and cupric oxide nano line is resistance to
Long property is stronger, is not easily broken or peels off, can be widely applied to the fields such as biosensing device, novel photoelectric-detection.
Compared with prior art, outstanding advantages of the invention are as follows：
1) two-dimensional structure for utilizing laser surface texture technology special in copper sheet Surface Texture, realizes controllable array micron knot
Structure；
2) thermal oxidation method growth oxidation copper nano-wire is used, a micro-nano compound structure is provided on copper sheet surface；
3) using the special two-dimensional structure in copper sheet surface as substrate, the thermal stress of cupric oxide nano line film can be reduced, make oxygen
Change copper nano-wire to be unlikely to be peel off；
4) heating temperature is 300~600 DEG C, and heating time is 3~5h, carries out open heating on hot plate.
Description of the drawings
Fig. 1 is cupric oxide nano line super hydrophobic surface composite construction preparation process schematic diagram.
Fig. 2 is grid type laser scan pattern.
Fig. 3 is oblique line formula laser scan pattern.
Fig. 4 is brickwall laser scan pattern.
Fig. 5 is laser galvanometer scanning system.
Specific implementation mode
Following embodiment will the present invention is further illustrated in conjunction with attached drawing.
Step 1, pending copper sheet (purity 99.96%, thickness 0.2mm) is placed in ultrasonic washing instrument, is used
The deionized water that resistivity is 18.25M Ω floods copper sheet surface, is cleaned by ultrasonic 2min, the copper sheet sample cleaned up is put into
It impregnates in the dilute hydrochloric acid of a concentration of 2mol/L, is cleaned again with absolute ethyl alcohol after taking-up, compressed nitrogen is used after cleaning up
Copper sheet is dried up, obtains copper sheet sample clean in Fig. 1 1.；
Step 2,1. laser surface texture is carried out to the clean copper sheet sample obtained described in step 1 using optical fiber laser,
2. texture pattern obtains copper sheet in Fig. 2 after laser texturing as shown in Figure 1, form micro-structure on copper sheet surface；It also can be such as Fig. 3
With the form of texture multiple patterns shown in Fig. 4；As shown in figure 5, the laser galvanometer scanning system is by optical fiber laser 1, attenuator
2, beam expander 3, galvanometer scanner 4, fθLens 5, the composition of hoistable platform 6 (containing sample)；
Step 3,2. the copper sheet after the texture obtained described in step 2 is placed in ultrasonic washing instrument, is flooded with absolute ethyl alcohol
Do not have copper sheet surface, be cleaned by ultrasonic 5min, 3min, subsequent naturally dry are rinsed with deionized water after taking-up；
Step 4, the copper sheet after drying will be cleaned described in step 3 2. to place on hot plate, temperature of heating plate is controlled 500
DEG C, heated at constant temperature 3h, room temperature is slowly dropped to after the completion of heating by copper sheet in air, the copper surface micro-structure described in step 2
On obtain micro-nano compound structure cupric oxide nano line as described in Figure 1 3.；
Step 5, the copper sheet obtained described in step 4 is immersed in stearic acid ethanol solution and impregnates 2h, naturally dry after taking-up,
It can obtain the super hydrophobic surface of cupric oxide nano line micro-nano compound structure.
The specific implementation mode of the present invention is above are only, but the design concept of the present invention is not limited thereto.
Claims (6)
1. a kind of super-hydrophobic composite construction preparation method of cupric oxide nano line, it is characterised in that include the following steps：
1) cleaning treatment is carried out to copper sheet surface；
2) Surface Texture is carried out to copper sheet using laser, micro-structure is formed on copper sheet surface；
3) cleaning treatment is carried out to the copper sheet after step 2) Surface Texture；
4) copper sheet after cleaning treatment is heated, then copper sheet is cooled to room temperature, micro-nano compound structure oxygen is obtained on copper sheet surface
Change copper nano-wire；
5) micro-nano compound structure cupric oxide nano line is modified using low-surface-energy material, copper oxide is obtained after drying and is received
The super hydrophobic surface of rice noodles micro-nano compound structure.
2. a kind of super-hydrophobic composite construction preparation method of cupric oxide nano line as described in claim 1, it is characterised in that in step
It is rapid 1) in, it is described to copper sheet surface carry out cleaning treatment specific method be：Copper sheet sample is positioned over and fills deionized water
It is cleaned in ultrasonic washing instrument, the copper sheet sample cleaned up is put into after being impregnated in dilute hydrochloric acid and is taken out, then with anhydrous second
Alcohol cleans, and compressed nitrogen is used in combination to dry up, and obtains clean copper sheet sample.
3. a kind of super-hydrophobic composite construction preparation method of cupric oxide nano line as described in claim 1, it is characterised in that in step
It is rapid 2) in, it is described using laser to copper sheet carry out Surface Texture, copper sheet surface formed micro-structure specific method be：Using swash
Optical surface texture technology carries out laser scanning processing after regulating optical fiber laser related processing parameters to clean copper sheet surface,
Special two-dimensional structure is processed on copper sheet surface, realizes controllable array micrometer structure.
4. a kind of super-hydrophobic composite construction preparation method of cupric oxide nano line as described in claim 1, it is characterised in that in step
It is rapid 3) in, the specific method that copper sheet after the Surface Texture to step 2) carries out cleaning treatment is：By step 2) Surface Texture
Copper sheet afterwards is cleaned by ultrasonic in ethyl alcohol, is dried up with compressed nitrogen after then being rinsed with deionized water.
5. a kind of super-hydrophobic composite construction preparation method of cupric oxide nano line as described in claim 1, it is characterised in that in step
It is rapid 4) in, the copper sheet by after cleaning treatment heats, then copper sheet is cooled to room temperature, and micro-nano composite junction is obtained on copper sheet surface
Structure cupric oxide nano line specific method is：Oxidation copper nano-wire is grown using thermal oxidation method, a micro-nano is provided on copper sheet surface
Composite construction；Using the special two-dimensional structure in copper sheet surface as substrate, reduces the thermal stress of cupric oxide nano line film, copper oxide is made to receive
Rice noodles film is not easily susceptible to cracking or peels off.
6. a kind of super-hydrophobic composite construction preparation method of cupric oxide nano line as described in claim 1, it is characterised in that in step
It is rapid 4) in, the heating is to carry out open heating on hot plate, and the temperature of heating is 300~600 DEG C, and the time of heating is
3~5h.
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| CN201810391335.9A CN108504984A (en) | 2018-04-27 | 2018-04-27 | A kind of super-hydrophobic composite construction preparation method of cupric oxide nano line |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109794686A (en) * | 2019-03-19 | 2019-05-24 | 北京理工大学 | Femtosecond laser enhances thermal oxidation process and prepares multifunctional electrodes |
| CN110508280A (en) * | 2019-09-06 | 2019-11-29 | 厦门大学 | The cupric oxide nano line and the preparation method and application thereof of the micro- texture foam copper of laser |
| CN111517357A (en) * | 2020-04-30 | 2020-08-11 | 鞍钢股份有限公司 | Preparation method of hydrophobic copper oxide nanosheet |
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| CN105514406A (en) * | 2016-02-23 | 2016-04-20 | 陕西科技大学 | Method for producing copper oxide nanowire array under room temperature |
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| CN101531335A (en) * | 2009-04-08 | 2009-09-16 | 西安交通大学 | Method for preparing metal surface superhydrophobic microstructure by femto-second laser |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109794686A (en) * | 2019-03-19 | 2019-05-24 | 北京理工大学 | Femtosecond laser enhances thermal oxidation process and prepares multifunctional electrodes |
| CN110508280A (en) * | 2019-09-06 | 2019-11-29 | 厦门大学 | The cupric oxide nano line and the preparation method and application thereof of the micro- texture foam copper of laser |
| CN111517357A (en) * | 2020-04-30 | 2020-08-11 | 鞍钢股份有限公司 | Preparation method of hydrophobic copper oxide nanosheet |
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Application publication date: 20180907 |