CN102976754A - Method for preparing carbon super-hydrophobic ceramic by sintering super-hydrophobic plant leaves - Google Patents
Method for preparing carbon super-hydrophobic ceramic by sintering super-hydrophobic plant leaves Download PDFInfo
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- CN102976754A CN102976754A CN2012105251308A CN201210525130A CN102976754A CN 102976754 A CN102976754 A CN 102976754A CN 2012105251308 A CN2012105251308 A CN 2012105251308A CN 201210525130 A CN201210525130 A CN 201210525130A CN 102976754 A CN102976754 A CN 102976754A
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Abstract
The invention relates to a method for preparing carbon super-hydrophobic ceramic by sintering super-hydrophobic plant leaves, which is characterized in that super-hydrophobic plant leaves are used as preparation templates, are sintered under the protection of a non-oxidizing atmosphere and are modified with fluorosilane low-surface-energy substances, thus preparing the carbon super-hydrophobic ceramic having a plant leaf surface structure. The method comprises the following steps: baking and drying lotus leaves, bamboo leaves, rice leaves and other super-hydrophobic plant leaves in a baking oven at 70-120 DEG C for 24-72 hours; placing the dried plant leaves in a sintering furnace having a non-oxidizing atmosphere such as argon gas, nitrogen gas and the like, and sintering to a temperature higher than 400 DEG C at a heating rate less than 5 DEG C/min, thus preparing the carbon ceramic having a plant leaf microscopic structure; and soaking the carbon ceramic in a fluorosilane and isopropanol mixed solution for more than 3 days, taking out, and airing. According to the invention, the prepared carbon super-hydrophobic ceramic well keeps the plant leaf microscopic structure, highly imitates the nature and has excellent super-hydrophobic property.
Description
Technical field
The invention belongs to a kind of method for preparing the super-hydrophobic pottery of carbon element, particularly a kind of method of utilizing the sintering plant leaf to prepare the super-hydrophobic pottery of carbon element.
Background technology
In the productive life, a lot of device parts are exposed in many dirt, Duo Shui, the multicontaminated environment throughout the year, be stained with difficult cleaning behind dust, aqueous vapor or the impurity, and can affect the performance of device component function, therefore people wish that also these device parts have super-hydrophobicity (spending greater than 150 with the contact angle of water), thereby realize self-cleaning function.The blade of a lot of plants of occurring in nature has super-hydrophobic ability, such as lotus leaf, Rice Leaf, Folium Arachidis hypogaeae, palm leaf, wild cabbage, taro leaves, China aster leaf etc.Scrutinize these blades, there are a lot of meticulous micro-nano projections on its surface and rough.When rainwater drops on these blades, rainwater only contacts with raised tip point, and the surface adhesion reactive force is very weak.Therefore the water globule that under surface tension effects, can congeal into, and can arbitrarily roll at blade surface.And dust also is that point contacts with blade, and the surface adhesion reactive force is little, is easy to be taken away by the globule.Super-hydrophobicity that the blades such as lotus leaf have utilized this micro-nano protruding constitution realization just, thus play self-cleaning effects.People imitate the structure of plant leaf usually at present, process uneven surface at the low surface energy material, or process uneven surface at the device parts first, and modify uneven surface with the low surface energy material, thereby make it have super-hydrophobic ability.Nowadays people have utilized sol-gel method, hydrothermal method, anonizing, Cement Composite Treated by Plasma, phase separation method, template-based extrusion method, electrochemical deposition method etc. to prepare the super hydrophobic materials such as the carbon of multiple coarse structure, zinc oxide, silicon oxide, titanium oxide.These materials can be used for the outdoor glass of high buildings and large mansions, vehicle glass, oil pipeline, outfall sewer, solar panel, outdoor antenna, blood compatibility biological material, boats and ships housing, fuel cell etc.Yet, the acquisition of these coarse structures is still by pure artificial imitation, even people adopt technology and the instrument of present highest level, still be difficult to copy out the fine structures that lotus leaf etc. was optimized through 1 years, this has also limited the further raising of material hydrophobic performance.Recently, people also copy plant leaf by lithography (or claiming the nanometer teeming practice) and construct to obtain super hydrophobic surface, namely utilize plant leaf as mother matrix, first coated dimethyl siloxane or metallic nickel on blade are removed the former that obtains the convex-concave inverse structure behind the blade; Again former is impressed on fluid polymer, or at former top casting fluid polymer, after polymer cure, remove former and can obtain the super-hydrophobic polymer surfaces similar with blade construction, details are referring to Artificial lotus leaf by nanocasting, Langmuir, 2005,21,8978-8981; Seung-Mo Le, Tai Hun Kwon, Mass-producible replication of highly hydrophobic surfaces from plant leaves, Nanotechnology, 2006,17,3189; Bin Liu, Yin Fan, Yaning He, Xiaogong Wang, Fabricating Super-Hydrophobic Lotus-Leaf-Like Surfaces through Soft-Lithographic Imprinting, Macromolecular Rapid Communications, 2006,27,1859.Because lithography needs to copy the surface that reprint just can obtain to have blade structure through twice, its surface structure is yielding in the multiple copies process, and fidelity is not high.Some complicated structures also are difficult to copy by printing means in the blade.And the reprint method needs to flow, curable material carries out the mold filling reprint, so this method can only obtain the super hydrophobic material of polymkeric substance, but is difficult to obtain ceramic super hydrophobic material.
Summary of the invention
The object of the present invention is to provide a kind of high level to use for reference the method for preparing the super-hydrophobic pottery of carbon element of nature, finished product excellent property.
The technical solution that realizes the object of the invention is: a kind ofly prepare the method for the super-hydrophobic pottery of carbon element with sintering super-hydrophobicity plant leaf, step is as follows:
(1) take the super-hydrophobicity plant leaf as raw material, is dried;
(2) dried plant leaf is placed non-oxidizing atmosphere protection sintering oven sintering, sintering temperature is greater than 400 ℃, and temperature rise rate is lower than 5 ℃/min, makes the carbon element pottery with plant leaf microtexture;
(3) the carbon element pottery being put into Virahol and silicon fluoride mixed solution soaked greater than 3 days;
(4) pottery of the carbon element after will soaking takes out dryly, just makes the super-hydrophobic pottery of the carbon element with plant leaf microtexture.
Drying described in the step 1 adopts in air natural drying or the baking oven baking dry, and described storing temperature is 70～120 ℃, and described baking time of drying is 24～72 hours; The preferred lotus leaf of described super-hydrophobicity plant leaf, Rice Leaf or rice-pudding leaf etc.
Non-oxidizing atmosphere described in the step 2 is argon gas or nitrogen; The preferred 500-800 of described sintering temperature ℃, preferred 1～2 ℃/min of temperature rise rate.
Silicon fluoride accounts for 10%～20% volume fraction in Virahol described in the step 3 and the silicon fluoride mixed solution, preferred 5～7 days of described soak time.
Principle of the present invention is: the present invention utilizes the super-hydrophobicity plant leaf to be template, with its sintering in non-oxidizing atmosphere.Organism during sintering in the blade decomposes, oxygen, hydrogen, nitrogen and part carbon change gaseous volatilization into, most carbons wherein then remain, and the micro-nano projection of blade surface is configured in the sintering process and also is retained, thereby forms the carbon element pottery with plant leaf microtexture.In the immersion process, hydrolysis and polycondensation occur to this carbon element pottery in silicon fluoride in the silicon fluoride solution of low surface energy, thereby at carbon element ceramic surface formation silicon fluoride self-assembled film as thin as a wafer.When water drops on this carbon element pottery, the air in the micro-nano protruding gap can be locked, forms one deck gas cloud as thin as a wafer between water and the carbon element pottery, and water only contacts with raised tip formation like this, and the surface adhesion reactive force is very weak.Therefore the water globule that under surface tension effects, can congeal into, thus realize super-hydrophobicity.
The present invention compared with prior art, its remarkable advantage: the super-hydrophobic pottery of prepared carbon element can be left over the microtexture of plant leaf better, the reference nature of higher degree has excellent ultra-hydrophobicity.
Below in conjunction with accompanying drawing the present invention is described in further detail.
Description of drawings
Fig. 1 is the XRD figure spectrum of utilizing the super-hydrophobic pottery of carbon element that the sintering lotus leaf makes in the embodiment of the invention 1.
Fig. 2 is the microtexture figure that utilizes the super-hydrophobic pottery of carbon element that the sintering lotus leaf makes in the embodiment of the invention 1.
Fig. 3 is the contact angle figure that utilizes the super-hydrophobic pottery of carbon element that the sintering lotus leaf makes in the embodiment of the invention 1.
Fig. 4 is the XRD figure spectrum of utilizing the super-hydrophobic pottery of carbon element that sintering rice-pudding leaf makes in the embodiment of the invention 2.
Fig. 5 is the microtexture figure that utilizes the super-hydrophobic pottery of carbon element that sintering rice-pudding leaf makes in the embodiment of the invention 2.
Fig. 6 is the contact angle figure that utilizes the super-hydrophobic pottery of carbon element that sintering rice-pudding leaf makes in the embodiment of the invention 2.
Fig. 7 is the XRD figure spectrum of utilizing the super-hydrophobic pottery of carbon element that the sintering Rice Leaf makes in the embodiment of the invention 3.
Fig. 8 is the microtexture figure that utilizes the super-hydrophobic pottery of carbon element that the sintering Rice Leaf makes in the embodiment of the invention 3.
Fig. 9 is the contact angle figure that utilizes the super-hydrophobic pottery of carbon element that the sintering Rice Leaf makes in the embodiment of the invention 3.
Embodiment
Prepare the method for the super-hydrophobic pottery of carbon element with plant leaf, its step is as follows:
(1) lotus leaf, rice-pudding leaf or Rice Leaf super-hydrophobicity plant leaf are toasted drying in baking oven, storing temperature is 70～120 ℃, and be 24～72 hours time of drying;
(2) dried plant leaf is placed the non-oxidizing atmosphere sintering oven sintering such as argon gas or nitrogen, make the carbon element pottery with plant leaf microtexture, sintering temperature is 500～800 ℃, and temperature rise rate is 1～2 ℃/min;
(3) the carbon element pottery was soaked 5～7 days in silicon fluoride and Virahol mixed solution, the silicon fluoride volume fraction is 10%～20% in the mixed solution;
(4) pottery of the carbon element after will soaking takes out and dries, and just makes the super-hydrophobic pottery of the carbon element with plant leaf microtexture.
Embodiment 1
Place the baking of 100 ℃ of baking ovens after dry 48 hours on lotus leaf, place the argon gas atmosphere stove to be heated to 200 ℃ with 2 ℃/minute temperature rise rate, be heated to 800 ℃ with 1 ℃/minute temperature rise rate again, make the carbon element pottery with lotus leaf microtexture.Figure 1 shows that the X diffracting spectrum that makes pottery, from the steamed bun shape diffraction peak of 22-26 ° of appearance as can be known the gained pottery be carbon.Figure 2 shows that the stereoscan photograph of the carbon element pottery microtexture that makes, visible carbon element pottery has been left over the microtexture of the micro-nano projection of lotus leaf surface well, and this structure has ultra-hydrophobicity for the carbon element pottery and plays a key effect.Again with this carbon element pottery after concentration is to soak 6 days in 20% the silicon fluoride solution, taking-up is dried, and just makes the super-hydrophobic pottery of the carbon element with lotus leaf microtexture.When water drops on this carbon element pottery, the air in the micro-nano protruding gap can be locked, forms the skim air film between water and the carbon element pottery, and water contacts with raised tip point like this, and the surface adhesion reactive force is very weak.Therefore the water globule that under surface tension effects, can congeal into, thus realize super-hydrophobicity.Figure 3 shows that the contact angle of the super-hydrophobic pottery of the carbon element that makes and water, θ
Contact angle=158 °, reach super-hydrophobicity.
Embodiment 2
Place the baking of 120 ℃ of baking ovens after dry 24 hours on rice-pudding leaf, place the nitrogen atmosphere stove to be heated to 600 ℃ with 2 ℃/minute temperature rise rate, make the carbon element pottery with rice-pudding leaf microtexture.Figure 4 shows that make the pottery the X diffracting spectrum, from steamed bun shape diffraction peak as can be known the gained pottery be carbon.Figure 5 shows that the stereoscan photograph of the carbon element pottery microtexture that makes, visible carbon element pottery has been left over the microtexture of the micro-nano projection of rice-pudding leaf surface well, and this structure has ultra-hydrophobicity for the carbon element pottery and plays a key effect.Again with the carbon element pottery after concentration is to soak 5 days in 15% the silicon fluoride solution, taking-up is dried, and just makes the super-hydrophobic pottery of carbon element with rice-pudding leaf microtexture.Figure 6 shows that the contact angle of the super-hydrophobic pottery of the carbon element that makes and water, θ
Contact angle=158 °, reach super-hydrophobicity.
Embodiment 3
Place the baking of 70 ℃ of baking ovens after dry 72 hours Rice Leaf, place the argon gas atmosphere stove to be heated to 500 ℃ with 2 ℃/minute temperature rise rate, make the carbon element pottery with Rice Leaf microtexture.Figure 7 shows that make the pottery the X diffracting spectrum, from steamed bun shape diffraction peak as can be known the gained pottery be carbon.Figure 8 shows that the stereoscan photograph of the carbon element pottery microtexture that makes, visible carbon element pottery has been left over the microtexture of Rice Leaf surface micronano projection well, and this structure has ultra-hydrophobicity for the carbon element pottery and plays a key effect.Again with the carbon element pottery after concentration is to soak 7 days in 10% the silicon fluoride solution, taking-up is dried, and just makes the super-hydrophobic pottery of the carbon element with Rice Leaf microtexture.Figure 9 shows that the contact angle of the super-hydrophobic pottery of the carbon element that makes and water, θ
Contact angle=159 °, reach super-hydrophobicity.
Claims (6)
1. a sintering super-hydrophobicity plant leaf prepares the method for the super-hydrophobic pottery of carbon element, it is characterized in that step is as follows:
Step 1, take the super-hydrophobicity plant leaf as raw material, be dried;
Step 2, dried plant leaf is placed non-oxidizing atmosphere protection sintering oven sintering, sintering temperature be greater than 400 ℃, and temperature rise rate is lower than 5 ℃/min, and it is ceramic to make the carbon element with plant leaf microtexture;
Step 3, the carbon element pottery is put into Virahol and silicon fluoride mixed solution soak greater than 3 days;
Step 4, the pottery of the carbon element after will soaking take out and dry, and just make the super-hydrophobic pottery of the carbon element with plant leaf microtexture.
2. sintering super-hydrophobicity plant leaf according to claim 1 prepares the method for the super-hydrophobic pottery of carbon element, it is characterized in that: in step 1, and the preferred lotus leaf of described super-hydrophobicity plant leaf, Rice Leaf or rice-pudding leaf.
3. sintering super-hydrophobicity plant leaf according to claim 1 prepares the method for the super-hydrophobic pottery of carbon element, it is characterized in that: in step 1, the described dry baking drying in air natural drying or the baking oven that adopts, described storing temperature is 70～120 ℃, and described baking time of drying is 24～72 hours.
4. sintering super-hydrophobicity plant leaf according to claim 1 prepares the method for the super-hydrophobic pottery of carbon element, it is characterized in that: in step 2, described non-oxidizing atmosphere is argon gas or nitrogen.
5. sintering super-hydrophobicity plant leaf according to claim 1 prepares the method for the super-hydrophobic pottery of carbon element, it is characterized in that: in step 2, and the preferred 500-800 of described sintering temperature ℃, preferred 1～2 ℃/min of temperature rise rate.
6. sintering super-hydrophobicity plant leaf according to claim 1 prepares the method for the super-hydrophobic pottery of carbon element, it is characterized in that: in step 3, silicon fluoride accounts for 10%～20% volume fraction in described Virahol and the silicon fluoride mixed solution, preferred 5～7 days of described soak time.
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Cited By (5)
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| CN105200528A (en) * | 2015-10-12 | 2015-12-30 | 南京理工大学 | Method for corrosively preparing silicon-base super-hydrophobic surface by utilizing pine structural porous silver as catalyst |
| CN106589435A (en) * | 2016-12-06 | 2017-04-26 | 南京理工大学 | Method for preparing epoxy resin surface with wood reverse structure |
| CN106591896A (en) * | 2016-12-06 | 2017-04-26 | 南京理工大学 | Method for preparing super-hydrophobic copper surface of plant leaf structure |
| CN108821257A (en) * | 2018-05-02 | 2018-11-16 | 福建农林大学 | A kind of binary based on lotus leaf is mesoporous-micropore multilevel structure biological carbon and its preparation method and application |
| CN110106534A (en) * | 2019-05-15 | 2019-08-09 | 南京理工大学 | A method of it prepares with the super-hydrophobic nickel surface of timber mirror surface structure |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105200528A (en) * | 2015-10-12 | 2015-12-30 | 南京理工大学 | Method for corrosively preparing silicon-base super-hydrophobic surface by utilizing pine structural porous silver as catalyst |
| CN105200528B (en) * | 2015-10-12 | 2017-08-04 | 南京理工大学 | Make the method that catalytic erosion prepares silicon substrate super hydrophobic surface using pine structural porous silver |
| CN106589435A (en) * | 2016-12-06 | 2017-04-26 | 南京理工大学 | Method for preparing epoxy resin surface with wood reverse structure |
| CN106591896A (en) * | 2016-12-06 | 2017-04-26 | 南京理工大学 | Method for preparing super-hydrophobic copper surface of plant leaf structure |
| CN106589435B (en) * | 2016-12-06 | 2019-06-21 | 南京理工大学 | A method of it prepares with timber reverse geometry epoxy resin surface |
| CN108821257A (en) * | 2018-05-02 | 2018-11-16 | 福建农林大学 | A kind of binary based on lotus leaf is mesoporous-micropore multilevel structure biological carbon and its preparation method and application |
| CN108821257B (en) * | 2018-05-02 | 2021-11-16 | 福建农林大学 | Lotus leaf-based binary mesoporous-microporous multilevel structure biochar and preparation method and application thereof |
| CN110106534A (en) * | 2019-05-15 | 2019-08-09 | 南京理工大学 | A method of it prepares with the super-hydrophobic nickel surface of timber mirror surface structure |
| CN110106534B (en) * | 2019-05-15 | 2021-03-26 | 南京理工大学 | Method for preparing super-hydrophobic nickel surface with wood mirror structure |
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Application publication date: 20130320 |