CN104944791A - Hot water non-stick surface structure and preparation method thereof - Google Patents
Hot water non-stick surface structure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a hot water non-stick surface structure and a preparation method thereof. The super-hydrophobic interface structure comprises a nano cone array structure formed on the surface of a substrate, wherein the nano array structure comprises a plurality of nano protrusions arranged in an array manner; at least the top of the nano protrusion is provided with a conical structure; the distance between two adjacent nano protrusions is 50-500nm; the top diameter of the nano protrusions is 1-200nm; and the surface of the nano array structure is modified with low surface energy substances. The preparation method is mainly implemented by virtue of a chemical bath deposition method. The super-hydrophobic surface structure disclosed by the invention has good hot water non-stick properties, non-stick impact and instantaneous rebound of hot water drops or hot water flow can be realized, the preparation process is easy to operate and control, any expensive equipment is not needed, and the super-hydrophobic surface structure is low in consumption, environment-friendly, high in reproducibility and short in period, can be prepared in large area and has excellent industrial application prospects.
Description
Technical field
The present invention relates to a kind of hydrophobic material, particularly a kind of hot water super-hydrophobic interface structure of not being stained with and preparation method thereof, belongs to material science.
Background technology
Usually, be greater than 150 ° of solid surface that simultaneously lagging angle is less than 10 ° with the contact angle of water and be considered to super-hydrophobic interface, super-hydrophobic interface has important value because it is applied in such as automatically cleaning, anticorrosion, Low Temperature Steam drop-wise condensation enhancement of heat transfer, anti-dewing, frosting resistance etc. in fundamental research and technology, causes the broad interest of academia and industry member.But when considering practical application, there is good application prospect at the super-hydrophobic interface that hot water is not stained with.The super hydrophobic surface that the such as type material of preparation solar heat protection scald, the surface design of hot water conveying pipe become hot water not to be stained with effectively can reduce energy consumption, the heat transfer of strengthening vapor condensation etc. by drag reduction.As everyone knows, high temperature water droplet has lower interfacial tension and stronger imbibition characteristic, and it sharply increased in the sticking of super-hydrophobic lotus leaf surface of classics, the super-hydrophobicity complete failure of lotus leaf surface when hot water temperature reaches 55 DEG C.In addition, bibliographical information is also had to have reduction in various degree through the anti-adversity of super hydrophobic surface to water that hot-water cure is crossed.Thus, the practical application of this super hydrophobic surface reduces greatly.
According to document " can superhydrophobic surfaces repel hot water " (J. Mater. Chem., 2009,19, p5602-5611) record, the hot water of the normal-temperature water of 25 DEG C and 55 DEG C drops in lotus leaf surface respectively, and the former is pearl at super-hydrophobic lotus leaf surface; But latter spreads over lotus leaf surface.The micro-nano compound structure observing the lotus leaf surface after hot-water cure in the secure execution mode (sem subsides; The document mentions hot water in addition has 160 ° to be down to about 80 ° at the contact angle of the super hydrophobic surface of its synthetic, and this super hydrophobic surface can not the shock of complete degeneration-resistant hot water as seen.
Not yet relate to hot water at present disclosed patent and be not stained with super hydrophobic surface, namely when hot water drips or hot water flow impinges upon super hydrophobic surface in static or dynamic mode and still maintains and be not stained with super-hydrophobicity.
Summary of the invention
Super-hydrophobic interface structure that the object of the present invention is to provide a kind of hot water not to be stained with and preparation method thereof, to overcome deficiency of the prior art.
For achieving the above object, present invention employs following technical scheme:
The super-hydrophobic interface structure that a kind of hot water is not stained with, comprise the nano array structure being formed at substrate surface, described nano array structure comprises the plural nanometer projection of array arrangement, and at least described nanometer projecting tip has cone structure, distance wherein between adjacent nano projection is at 50 ~ 500 nm, the top diameter of described nanometer projection is 1 ~ 200 nm, and described nano array structure surface is also modified with low-surface energy substance simultaneously.
The preparation method of the super-hydrophobic interface structure that former hotter water is not stained with comprises:
(1), after substrate surface being cleaned, dry up for subsequent use with the gas do not reacted with base material;
(2) substrate after step (1) process is placed in reaction solution, and reaction solution is heated to 25 ~ 100 DEG C, insulation more than 5min, thus growth forms described nano array structure on the bottom face of described substrate, described reaction solution is the soluble Zn source material of 1:6 ~ 1:10 and the uniform solution of soluble alkali materials containing mol ratio;
(3) in step (2) the nano array structure finishing low-surface energy substance that obtains, the super-hydrophobic interface structure that described hot water is not stained with is formed.
Further, abovementioned steps (1) comprising: use acetone, ethanol and each more than the 15min of deionized water ultrasonic cleaning base material successively, and dry up with the gas do not reacted with base material subsequently, the described gas do not reacted with base material comprises pure nitrogen gas.
Further, abovementioned steps (2) comprising: the alkaline substance solution be the zinc source material aqueous solution and the concentration of 0.1mM ~ 5M by concentration being 0.1mM ~ 5M mixes, and accompanies by stirring simultaneously, avoids occurring precipitation, thus form the reaction solution of transparent and homogeneous.
Further, described nanometer projection comprises zinc-oxide nano cone or zinc-oxide nano pencil-shaped projection.
Further, described substrate can be selected from but be not limited to copper material, can also be the substrate of modifying crystal seed, as glass, macromolecular material etc.
Further, described low-surface energy substance can be selected from but be not limited to the combination of any one or more in silicon fluoride, siloxanes, tetrafluoroethylene, silane coupling agent, higher fatty acid.
Further, aforementioned base material can be selected from but be not limited to the combination of any one or more in potassium hydroxide, sodium hydroxide, sodium carbonate, sodium bicarbonate, salt of wormwood, saleratus, ammoniacal liquor, urea.
Further, described zinc source material can be selected from but be not limited to the combination of any one or more in zinc nitrate, zinc chloride, zinc sulfate, zinc phosphate, zinc acetate.
Further, abovementioned steps (3) comprising: the method selecting vapour deposition method, immersion-oven drying method or other industry known, in step (2) the nano array structure finishing low-surface energy substance that obtains, forms the super-hydrophobic interface structure that described hot water is not stained with.
Compared with prior art, beneficial effect of the present invention comprises:
(1) this super-hydrophobic interface structure has good hot water being not stained with property, with the contact angle of water more than 160 °, not being stained with of can realizing that hot water drips clash into and instantaneously bullet from, contribute to designing the protective material of novel solar heat protection scald, super-hydrophobic interface that less energy-consumption hot water transports surface, enforcing condensation heat transfer, can be applicable to many high-technology fields such as aerospace, nuclear energy, material, environmental engineering, new forms of energy and Agricultural engineering.
(2) the simple chemical bath growth method of preparation method system of super-hydrophobic interface structure be not stained with of this hot water, easy handling and regulation and control, without the need to any expensive device, low consumption environment protection, favorable reproducibility, the cycle is short, can big area prepare, and according to production-scale demand, get final product industrialization by suitably adjusting, there is good prospects for commercial application.
Accompanying drawing explanation
Fig. 1 a-Fig. 1 b be respectively the embodiment of the present invention 1,2 obtain zinc-oxide nano cone array and the structural representation of zinc-oxide nano pencil array, wherein: 11-substrate, 12-zinc-oxide nano cone array, 13-zinc-oxide nano pencil array;
Fig. 2 a-Fig. 2 b be respectively the embodiment of the present invention 1,2 obtain zinc-oxide nano cone array and the texture edge figure of zinc-oxide nano pencil array.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and the specific embodiments, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
But, in this manual, the such as relational terms of first and second grades and so on is only used for an entity or operation to separate with another entity or operational zone, and not necessarily requires or imply the relation that there is any this reality between these entities or operation or sequentially.And, term " comprises ", " comprising " or its any other variant are intended to contain comprising of nonexcludability, thus make to comprise the process of a series of key element, method, article or equipment and not only comprise those key elements, but also comprise other key elements clearly do not listed, or also comprise by the intrinsic key element of this process, method, article or equipment.When not more restrictions, by statement " comprising one ... " the key element limited, and be not precluded within process, method, article or the equipment comprising described key element and also there is other identical element.
One aspect of the present invention provides the super-hydrophobic interface structure that a kind of hot water is not stained with, it comprises the nano array structure being formed at substrate surface, described nano array structure comprises the plural nanometer projection of array arrangement, and at least described nanometer projecting tip has cone structure, distance wherein between adjacent nano projection is at 50 ~ 500 nm, the top diameter of described nanometer projection is 1 ~ 200 nm, and described nano array structure surface is also modified with low-surface energy substance simultaneously.
Further, aforementioned nanometer projection comprises zinc-oxide nano cone or zinc-oxide nano pencil-shaped projection.Wherein, zinc oxide, as a kind of direct band gap broadband semiconductor, has good chemical stability, is widely used at numerous areas such as new forms of energy, material and microelectronics.
Further, after zinc-oxide nano cone array surface modification of the present invention, show excellent hot water and be not stained with super-hydrophobic stability, in other words, when hot water drip impinge upon zinc oxide nano array surface time, can't infiltrate this surface in contact, this surface still maintains super-hydrophobicity.
Nano array structure of the present invention is actually nano-scale gap compact arranged collimation nanoneedle cone array, it not only can guarantee that noninfiltrated liquid-vapo(u)r interface is thermally-stabilised, and effectively can avoid the pining force of solid-solution-air three-phase line of contact, even if the hot water drop of differing temps sprawl instantaneously in violent knockout process also can rapidly bullet from, whole residence time, at about 10 ms, makes water droplet Yin Wendu raise and the effect of the low surface tension that brings and low fluid degree of being stained with is ignored.
The super-hydrophobic interface structure that hot water of the present invention is not stained with, or think that heat-staple super-hydrophobic interface can the shock that drips of degeneration-resistant hot water, contribute to designing the protective material of novel solar heat protection scald, super-hydrophobic interface that less energy-consumption hot water transports surface, enforcing condensation heat transfer.
Another aspect of the present invention provides a kind of method preparing the super-hydrophobic interface structure that former hotter water is not stained with, and it mainly utilizes chemical bath deposition method to realize, and comprises following key step: the pre-treatment of substrate surface; Chemical bath grows.By the regulation and control of the size controlling the material formula of growth media (or being called " reaction solution "), growth media concentration and the experiment condition such as temperature, growth time can realize nanostructure, pattern and density.
In a better embodiment, the preparation method of the super-hydrophobic interface structure that former hotter water is not stained with can comprise:
(1), after substrate surface being cleaned, dry up for subsequent use with the gas do not reacted with base material;
(2) substrate after step (1) process is placed in reaction solution, and reaction solution is heated to 25 ~ 100 DEG C, insulation more than 5min, thus growth forms described nano array structure on the bottom face of described substrate, described reaction solution is the soluble Zn source material of 1:6 ~ 1:10 and the uniform solution of soluble alkali materials containing mol ratio;
(3) in step (2) the nano array structure finishing low-surface energy substance that obtains, the super-hydrophobic interface structure that described hot water is not stained with is formed.
And in one more specifically embodiment, this preparation method can comprise:
The pre-treatment on the first step copper material surface, this step prepares the important step of nano array structure.Acetone, ethanol and each 15min of deionized water ultrasonic cleaning copper material are used in concrete operations successively.Subsequently with pure nitrogen gas or other gas do not reacted with copper material, such as rare gas element dries up, and prevents the excessively oxidated crystal seed on copper material surface that causes in its surface to be destroyed.
Second step chemical bath deposition process, this step is the key link realizing nano array structure controlled synthesis.Growth media formula, concentration and temperature and growth time are closely related with pattern to the size of nano array structure, density.Growth media is preferably the zine ion aqueous solution of 0.1mM ~ 5M concentration and the mixing formula of 0.1mM ~ 5M concentration basic solution, the volumetric molar concentration ratio of zine ion solution and basic solution controls at 1:6 ~ 1:1,5min ~ 180min is reacted in 25 ~ 100 ° of C water-baths, be preferably 30min ~ 3h, obtain nano array structure.
3rd step finishing, this step can adopt vapour deposition method modification that other also can be adopted to realize as first soaked the modifying method of post-drying.
Further, in this specific embodiments, this preparation method can prepare nano-array device by chemical bath growth method and realize.
Aforementioned substrates, low-surface energy substance, alkaline matter, zinc source material can be selected from but be not limited to listed all kinds of materials above.
Preparation method of the present invention belongs to chemical bath deposition method, it is one of the easiest method preparing film and nano material, simple to operate, do not rely on expensive equipment, and there is extensibility, be applicable to big area batch processing or successive sedimentation, the product stable obtained, evenly, strong adhesion and favorable reproducibility, the Modulatory character of reaction process and product form is high.
Technical scheme of the present invention is intuitively shown further below in conjunction with some representative embodiment.
embodiment 1
1.select that 2 mm commercially produced are thick, area about 4 cm
2glass 11, use acetone, ethanol, deionized water ultrasonic cleaning 15min successively.
Drying up with pure nitrogen gas avoids oxidized, places for subsequent use.
According to the volume ratio of 1:1,0.5M zinc nitrate aqueous solution is poured in 4M aqueous sodium hydroxide solution, stirs simultaneously, avoid the generation precipitated.Pre-treatment to be got well and the glass reverse side applying crystal seed puts into reaction solution upward, continues after being heated to 90 DEG C to keep this temperature 3h, zinc-oxide nano pencil array 13.
Finishing, this step can adopt vapour deposition method modification that other also can be adopted to realize as first soaked the modifying method of post-drying.Be specially sample to be finished to put into and be warming up to 120
oc, evaporation 2h takes out after being down to normal temperature.Or with the FAS alcohol solution dipping 2h of 2%, be then warming up to 80
oCbaking oven in constant temperature 1h, take out after being down to normal temperature.
Performance test.(1) qualitative discrimination: by 100
oc boiling water stream is cast in the sample surfaces of modified from the height of 3cm, find that current can bullet be from sample surfaces instantaneously, sample surfaces does not have water stain remaining.(2) quantitative identification: respectively by 25
oc, 50
oc, 70
oc, 90
othe hot water of the 8 μ L of C drips the sample surfaces impinging upon modified from the height of 3cm.Find that the water droplet experience of each temperature is dripped, sprawled, bullet is from a series of process.From the angle of quantitative and qualitative analysis, we prove that this super-hydrophobic nano array surface has hot water and is not stained with respectively.
embodiment 2
1.select the copper material 11 that the 8mm commercially produced is thick, area is about 4cm2, use acetone, ethanol, deionized water ultrasonic cleaning 15min successively.
Drying up with pure nitrogen gas avoids oxidized, places for subsequent use.
According to the volume ratio of 1:1,0.5M zinc nitrate aqueous solution is poured in 4M aqueous sodium hydroxide solution, stirs simultaneously, avoid the generation precipitated.Copper coin reverse side good for pre-treatment is put into reaction solution upward, after heating 60 DEG C continue keep this temperature 30min, zinc-oxide nano wimble structure 12.
Finishing, this step can adopt vapour deposition method modification that other also can be adopted to realize as first soaked the modifying method of post-drying.Be specially sample to be finished to put into and be warming up to 120
oc, evaporation 2h takes out after being down to normal temperature.Or with the FAS alcohol solution dipping 2h of 2%, be then warming up to 80
oCbaking oven in constant temperature 1h, take out after being down to normal temperature.
Performance test.(1) qualitative discrimination: by 100
oc boiling water stream is cast in the sample surfaces of modified from the height of 3cm, find that current can bullet be from sample surfaces instantaneously, sample surfaces does not have water stain remaining.(2) quantitative identification: respectively by 25
oc, 50
oc, 70
oc, 90
othe hot water of the 8 μ L of C drips the sample surfaces impinging upon modified from the height of 3cm.Find that the water droplet experience of each temperature is dripped, sprawled, bullet is from a series of process.From the angle of quantitative and qualitative analysis, we prove that this super-hydrophobic nano array surface has hot water and is not stained with respectively.
Should be appreciated that in addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of application claims.
Claims (10)
1. a hot water super-hydrophobic interface structure of not being stained with, it is characterized in that comprising the nano array structure being formed at substrate surface, described nano array structure comprises the plural nanometer projection of array arrangement, and at least described nanometer projecting tip has cone structure, distance wherein between adjacent nano projection is at 50 ~ 500 nm, the top diameter of described nanometer projection is 1 ~ 200 nm, and described nano array structure surface is also modified with low-surface energy substance simultaneously.
2. the hot water according to claim 1 super-hydrophobic interface structure of not being stained with, is characterized in that described nanometer projection comprises zinc-oxide nano cone or zinc-oxide nano pencil-shaped projection.
3. the hot water according to claim 1 super-hydrophobic interface structure of not being stained with, it is characterized in that described substrate comprises the substrate of copper material or coating crystal seed, the substrate of described coating crystal seed comprises glass or macromolecular material.
4. the hot water according to claim 1 super-hydrophobic interface structure of not being stained with, is characterized in that described low-surface energy substance comprises silicon fluoride, siloxanes, tetrafluoroethylene, silane coupling agent or higher fatty acid.
5. the preparation method of super-hydrophobic interface structure that is not stained with of hot water described in claim 1, is characterized in that comprising:
(1), after substrate surface being cleaned, dry up for subsequent use with the gas do not reacted with base material;
(2) substrate after step (1) process is placed in reaction solution, and reaction solution is heated to 25 ~ 100 DEG C, insulation more than 5min, thus growth forms described nano array structure on the bottom face of described substrate, described reaction solution is the soluble Zn source material of 1:6 ~ 1:10 and the uniform solution of soluble alkali materials containing mol ratio;
(3) in step (2) the nano array structure finishing low-surface energy substance that obtains, the super-hydrophobic interface structure that described hot water is not stained with is formed.
6. the preparation method of super-hydrophobic interface structure that is not stained with of hot water described in claim 5, it is characterized in that step (1) comprising: use acetone, ethanol and each more than the 15min of deionized water ultrasonic cleaning base material successively, dry up with the gas do not reacted with base material subsequently, the described gas do not reacted with base material comprises pure nitrogen gas.
7. the preparation method of super-hydrophobic interface structure that is not stained with of hot water described in claim 5, it is characterized in that, step (2) comprising: the alkaline substance solution be the zinc source material aqueous solution and the concentration of 0.1mM ~ 5M by concentration being 0.1mM ~ 5M mixes, accompany by stirring simultaneously, avoid occurring precipitation, thus form the reaction solution of transparent and homogeneous.
8. the preparation method of super-hydrophobic interface structure that is not stained with of hot water described in claim 5 or 7, is characterized in that described alkaline matter comprises potassium hydroxide, sodium hydroxide, sodium carbonate, sodium bicarbonate, salt of wormwood, saleratus, ammoniacal liquor or urea.
9. the preparation method of super-hydrophobic interface structure that is not stained with of hot water described in claim 5 or 7, is characterized in that described zinc source material comprises zinc nitrate, zinc chloride, zinc sulfate, zinc phosphate or zinc acetate.
10. the preparation method of super-hydrophobic interface structure that is not stained with of hot water described in claim 5, it is characterized in that, step (3) comprising: at least select vapour deposition method or immersion-oven drying method in step (2) the nano array structure finishing low-surface energy substance that obtains, form the super-hydrophobic interface structure that described hot water is not stained with;
Described low-surface energy substance comprises silicon fluoride, siloxanes, tetrafluoroethylene, silane coupling agent or higher fatty acid.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105463564A (en) * | 2015-11-30 | 2016-04-06 | 东南大学 | ZnO nanorod and ZnO cluster composite structure and preparation method thereof |
| CN105799168A (en) * | 2016-04-06 | 2016-07-27 | 南京增材制造研究院发展有限公司 | Continuous instantaneous exposure photocuring printer provided with anti-sticking resistance-reducing nano-structured tank bottom |
| CN106007794A (en) * | 2016-05-16 | 2016-10-12 | 北京航空航天大学 | Method for inducing wettability changes of super-hydrophobic film through solvent and application |
| CN106835079A (en) * | 2017-01-17 | 2017-06-13 | 江苏理工学院 | A kind of preparation method of anti-fog micro-nano compound structure copper substrate superhydrophobic surface |
| CN108570850A (en) * | 2018-02-15 | 2018-09-25 | 湖北大学 | A kind of preparation method of the excellent super wetting woven fabric of stabilization patience for water-oil separating |
| CN109467857A (en) * | 2018-10-19 | 2019-03-15 | 南京邮电大学 | A kind of zinc oxide/polytetrafluorethylenano nano composite material and preparation method |
| CN111876766A (en) * | 2020-07-14 | 2020-11-03 | 中国科学院海洋研究所 | Preparation method and application of super-hydrophobic surface for controlling liquid drop self-bounce effect |
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| CN105463564A (en) * | 2015-11-30 | 2016-04-06 | 东南大学 | ZnO nanorod and ZnO cluster composite structure and preparation method thereof |
| CN105799168A (en) * | 2016-04-06 | 2016-07-27 | 南京增材制造研究院发展有限公司 | Continuous instantaneous exposure photocuring printer provided with anti-sticking resistance-reducing nano-structured tank bottom |
| CN105799168B (en) * | 2016-04-06 | 2018-10-30 | 南京增材制造研究院发展有限公司 | A kind of continuous instantaneous exposure photocuring printer in anti-sticking drag-reduction nano structure grooves bottom |
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| CN106835079A (en) * | 2017-01-17 | 2017-06-13 | 江苏理工学院 | A kind of preparation method of anti-fog micro-nano compound structure copper substrate superhydrophobic surface |
| CN108570850A (en) * | 2018-02-15 | 2018-09-25 | 湖北大学 | A kind of preparation method of the excellent super wetting woven fabric of stabilization patience for water-oil separating |
| CN108570850B (en) * | 2018-02-15 | 2021-03-02 | 湖北大学 | Preparation method of super-wetting woven fabric with excellent stability and tolerance for oil-water separation |
| CN109467857A (en) * | 2018-10-19 | 2019-03-15 | 南京邮电大学 | A kind of zinc oxide/polytetrafluorethylenano nano composite material and preparation method |
| CN111876766A (en) * | 2020-07-14 | 2020-11-03 | 中国科学院海洋研究所 | Preparation method and application of super-hydrophobic surface for controlling liquid drop self-bounce effect |
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Application publication date: 20150930 |