CN102041535B - Method for preparing two types of super-hydrophobic membranes simultaneously by utilizing ferric chloride - Google Patents
Method for preparing two types of super-hydrophobic membranes simultaneously by utilizing ferric chloride Download PDFInfo
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- CN102041535B CN102041535B CN201010507958A CN201010507958A CN102041535B CN 102041535 B CN102041535 B CN 102041535B CN 201010507958 A CN201010507958 A CN 201010507958A CN 201010507958 A CN201010507958 A CN 201010507958A CN 102041535 B CN102041535 B CN 102041535B
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Abstract
The invention relates to a method for preparing two types of super-hydrophobic membranes simultaneously by utilizing ferric chloride, in particular to a method for preparing a copper myristate membrane with a micro/nano-structure and a myristic acid membrane embedded with iron particles. The method is technically characterized in that: the ferric chloride and myristic acid powder are dispersed in absolute ethanol to form uniform electrolyte, and two copper sheets with 60mm*25mm*1.5mm are taken as electrodes and are electrolyzed under certain direct-current voltage for a certain period of time, so that the copper myristate membrane with the micro/nano-structure is formed at an anode and the myristic acid membrane embedded with the iron particles is formed at a cathode. The invention provides a simple method for preparing super-hydrophobic membranes at the anode and the cathode simultaneously for the first time; and the super-hydrophobic membranes have good super-hydrophobic performance and have wide application prospect.
Description
Technical field
The present invention relates to a kind of method of utilizing two kinds of based superhydrophobic thin films that iron(ic)chloride prepares simultaneously, particularly the TETRADECONIC ACID copper film of micro and the method that is inlaid with iron particulate TETRADECONIC ACID film.
Background technology
Wettability is a very important index of solid surface, and it mainly can receive the chemical energy on surface and the influence of microtexture.Natural a lot of plant for example lotus leaf has all been showed extraordinary ultra thin performance, and usually all there is the structure of two kinds of yardsticks of micro-nano on the surface of these blades, and had low roll angle with can be up to the contact angle more than 150 °.The researchist is in theory and experimentally the structure of lotus leaf has been done a large amount of research.And from physics and chemical terms, about geometric scale, surfaceness and surface energy have carried out discussing widely to the influence of the wettability of ultraphobic surface.At present, mainly contain anodic oxidation, galvanic deposit, chemical corrosion, plasma etching, laser treatment, electric spinning, chemical vapour deposition, collosol and gel or the like about the method for preparing ultra thin material.But also there are some shortcomings in these methods, the for example material of exacting terms, costliness, special devices, the technology controlling and process of complicacy and the use of template, and these have all seriously hindered its large-scale application in engineering.Yet a kind of simple chemical process has been reported in river etc., adopts TETRADECONIC ACID solution soaking copper base to prepare ultra thin material, but type long and substrate of required cycle is limited.Therefore, adopt a kind of efficient, inexpensive, method will have remarkable advantages in the application of industrial big scale simply and easily.In addition, it should be noted that in the past all the preparation ultra thin material method in can only prepare a kind of ultra thin material film.
Summary of the invention
The technical problem that solves
For fear of the weak point of prior art, the present invention proposes a kind of method of utilizing two kinds of based superhydrophobic thin films that iron(ic)chloride prepares simultaneously, is based on the method that TETRADECONIC ACID/absolute ethyl alcohol/iron(ic)chloride composite electrolytic solution can prepare two kinds of super-drainage structure films simultaneously.
Thought of the present invention is: after iron(ic)chloride is dissolved in absolute ethyl alcohol fully; Under the condition of magnetic agitation, continue to add the TETRADECONIC ACID powder and make it to form the electrolytic solution that mixes; With the copper sheet of two 60mm * 25mm * 1.5mm as anode and negative electrode; The electrolysis regular hour under certain voltage, the TETRADECONIC ACID copper film of formation micro on anode; Be inlaid with iron particulate TETRADECONIC ACID film and on negative electrode, form, take out at last in zero(ppm) water after the cleaning many times, so just to have prepared two kinds of super-hydrophobic thin-film materials simultaneously in drying at room temperature.
Technical scheme
A kind of method of utilizing two kinds of based superhydrophobic thin films that iron(ic)chloride prepares simultaneously is characterized in that step is following:
Step 1: place absolute ethyl alcohol to make it to dissolve fully in iron(ic)chloride, form uniform solution, the iron(ic)chloride add-on is 0.02mol/L～0.08mol/L;
Step 2: with molar mass is that the TETRADECONIC ACID powder of 0.08mol/L～0.5mol/L is dispersed in the above-mentioned solution under the condition of magnetic agitation, makes it to mix formation electrolytic solution;
Step 3: in electrolytic solution, put into two copper sheets as anode and negative electrode, the volts DS that between anode and negative electrode, loads 15～30V carries out electrolysis, and electrolysis time is 10min～30min;
Step 4: after electrolysis is accomplished, anode and negative electrode are cleaned in zero(ppm) water afterwards in drying at room temperature, obtain the TETRADECONIC ACID copper film of micro, obtain being inlaid with the TETRADECONIC ACID iron thin film of ferric oxide particles at negative electrode at anode.
Described two copper sheet size 60mm * 25mm * 1.5mm.
The contact angle of negative electrode and anode copper sheet all is transformed into super-hydrophobicity from wetting ability and reaches 160 °, and roll angle is less than 2 °.
Beneficial effect
A kind of method of utilizing two kinds of based superhydrophobic thin films that iron(ic)chloride prepares simultaneously that the present invention proposes; Adopt TETRADECONIC ACID and iron(ic)chloride material to come preparing electrolyte; Relate to two kinds of based superhydrophobic thin films that adopt a kind of simple electrochemical method in the copper sheet substrate, can prepare simultaneously, and these two kinds of films all have great contact angle and less roll angle with micro.It is the method that to prepare two kinds of different ultra thin thin-film materials with a kind of simple method simultaneously.
Description of drawings
Fig. 1 is for adding 2g FeCl
36H
2The 0.08M/L TETRADECONIC ACID of O is at the sem photograph of voltage 15V electrolysis time 15min; A: anode sem photograph; B: negative electrode sem photograph
Fig. 2 is for adding 2g FeCl
36H
2The 0.5M/L TETRADECONIC ACID of O is at the sem photograph of voltage 15V electrolysis time 15min; A: anode sem photograph; B: negative electrode sem photograph
Fig. 3 is for adding 2g FeCl
36H
2The 0.5M/L TETRADECONIC ACID of O is at the sem photograph of voltage 30V electrolysis time 15min; A: anode sem photograph; B: negative electrode sem photograph
Fig. 4 is for adding 1g FeCl
36H
2The 0.5M/L TETRADECONIC ACID of O is at the sem photograph of voltage 15V electrolysis time 30min; A: anode sem photograph; B: negative electrode sem photograph
Fig. 5 is for adding 2g FeCl
36H
2The 0.5M/L TETRADECONIC ACID of O is at the sem photograph of voltage 15V electrolysis time 30min; A: anode sem photograph; B: negative electrode sem photograph
Fig. 6 is for adding 2g FeCl
36H
2The 0.5M/L TETRADECONIC ACID of O is at the sem photograph of voltage 15V electrolysis time 10min; A: anode sem photograph; B: negative electrode sem photograph
Fig. 7 is for adding 2g FeCl
36H
2The 0.08M/L stearic acid of O is at the sem photograph of voltage 15V electrolysis time 15min; A: anode sem photograph; B: negative electrode sem photograph
Embodiment
Combine embodiment, accompanying drawing that the present invention is further described at present:
The present invention is raw materials used to be had: commercially available absolute ethyl alcohol; The iron(ic)chloride analytical pure; TETRADECONIC ACID; 60mm * 25mm * 1.5mm copper sheet; Zero(ppm) water; Waterproof abrasive paper.
Embodiment one
At first with 2g FeCl
36H
2O places the 150ml absolute ethyl alcohol to make it to dissolve fully, forms uniform solution; Secondly 2.741g TETRADECONIC ACID powder is dispersed in the above-mentioned solution under the condition of magnetic agitation, makes it to mix, contain the TETRADECONIC ACID electrolytic solution of 0.08mol/l with formation.Then will be in advance place electrolyzer with the copper sheet of the liquid honing of 400 and 800 granularities and two 60mm * 25mm * 1.5mm drying up; And above-mentioned electrolytic solution poured in the electrolyzer; Electrolysis under the volts DS of 15V; The based superhydrophobic thin films that on anode and negative electrode, forms behind the electrolysis 15min is seen Fig. 1, and concrete contact angle is seen table 1.
Embodiment two
At first with 2g FeCl
36H
2O places the 150ml absolute ethyl alcohol to make it to dissolve fully, forms uniform solution; Secondly 17.125g TETRADECONIC ACID powder is dispersed in the above-mentioned solution under the condition of magnetic agitation, makes it to mix, contain the TETRADECONIC ACID electrolytic solution of 0.5mol/l with formation.Then will be in advance place electrolyzer with the copper sheet of the liquid honing of 400 and 800 granularities and two 60mm * 25mm * 1.5mm drying up; And above-mentioned electrolytic solution poured in the electrolyzer; Electrolysis under the volts DS of 15V; The based superhydrophobic thin films that on anode and negative electrode, forms behind the electrolysis 15min is seen Fig. 2, and concrete contact angle is seen table 1.
Embodiment three
At first with 2g FeCl
36H
2O places the 150ml absolute ethyl alcohol to make it to dissolve fully, forms uniform solution; Secondly 17.125g TETRADECONIC ACID powder is dispersed in the above-mentioned solution under the condition of magnetic agitation, makes it to mix, contain the TETRADECONIC ACID electrolytic solution of 0.5mol/l with formation.Then will be in advance place electrolyzer with the copper sheet of the liquid honing of 400 and 800 granularities and two 60mm * 25mm * 1.5mm drying up; And above-mentioned electrolytic solution poured in the electrolyzer; Electrolysis under the volts DS of 30V; The based superhydrophobic thin films that on anode and negative electrode, forms behind the electrolysis 15min is seen Fig. 3, and concrete contact angle is seen table 1.
Embodiment four
At first with 1g FeCl
36H
2O places the 150ml absolute ethyl alcohol to make it to dissolve fully, forms uniform solution; Secondly 17.125g TETRADECONIC ACID powder is dispersed in the above-mentioned solution under the condition of magnetic agitation, makes it to mix, contain the TETRADECONIC ACID electrolytic solution of 0.5mol/l with formation.Then will be in advance place electrolyzer with the copper sheet of the liquid honing of 400 and 800 granularities and two 60mm * 25mm * 1.5mm drying up; And above-mentioned electrolytic solution poured in the electrolyzer; Electrolysis under the volts DS of 15V; The based superhydrophobic thin films that on anode and negative electrode, forms behind the electrolysis 30min is seen Fig. 4, and concrete contact angle is seen table 1.
Embodiment five
At first with 2g FeCl
36H
2O places the 150ml absolute ethyl alcohol to make it to dissolve fully, forms uniform solution; Secondly 17.125g TETRADECONIC ACID powder is dispersed in the above-mentioned solution under the condition of magnetic agitation, makes it to mix, contain the TETRADECONIC ACID electrolytic solution of 0.5mol/l with formation.Then will be in advance place electrolyzer with the copper sheet of the liquid honing of 400 and 800 granularities and two 60mm * 25mm * 1.5mm drying up; And above-mentioned electrolytic solution poured in the electrolyzer; Electrolysis under the volts DS of 15V; The based superhydrophobic thin films that on anode and negative electrode, forms behind the electrolysis 30min is seen Fig. 5, and concrete contact angle is seen table 1.
Embodiment six
At first with 2g FeCl
36H
2O places the 150ml absolute ethyl alcohol to make it to dissolve fully, forms uniform solution; Secondly 17.125g TETRADECONIC ACID powder is dispersed in the above-mentioned solution under the condition of magnetic agitation, makes it to mix, contain the TETRADECONIC ACID electrolytic solution of 0.5mol/l with formation.Then will be in advance place electrolyzer with the copper sheet of the liquid honing of 400 and 800 granularities and two 60mm * 25mm * 1.5mm drying up; And above-mentioned electrolytic solution poured in the electrolyzer; Electrolysis under the volts DS of 15V; The based superhydrophobic thin films that on anode and negative electrode, forms behind the electrolysis 10min is seen Fig. 6, and concrete contact angle is seen table 1.
Embodiment seven
At first with 2g FeCl
36H
2O places the 150ml absolute ethyl alcohol to make it to dissolve fully, forms uniform solution; Secondly 3.414g TETRADECONIC ACID powder is dispersed in the above-mentioned solution under the condition of magnetic agitation, makes it to mix, contain the TETRADECONIC ACID electrolytic solution of 0.08mol/l with formation.Then will be in advance place electrolyzer with the copper sheet of the liquid honing of 400 and 800 granularities and two 60mm * 25mm * 1.5mm drying up; And above-mentioned electrolytic solution poured in the electrolyzer; Electrolysis under the volts DS of 15V; The based superhydrophobic thin films that on anode and negative electrode, forms behind the electrolysis 15min is seen Fig. 7, and concrete contact angle is seen table 1.
Table 1: the contact angle of embodiment sample
| Sample | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 |
| The anode contact angle (°) | 161 | 147 | 152 | 162 | 142 | 162 | 141 |
| The negative electrode contact angle (°) | 163 | 163 | 163 | 145 | 162 | 163 | 163 |
Claims (3)
1. method of utilizing two kinds of based superhydrophobic thin films that iron(ic)chloride prepares simultaneously is characterized in that step is following:
Step 1: place absolute ethyl alcohol to make it to dissolve fully in iron(ic)chloride, form uniform solution, the iron(ic)chloride add-on is 0.02mol/L～0.08mol/L;
Step 2: the TETRADECONIC ACID powder is dispersed in the above-mentioned solution under the condition of magnetic agitation, makes it to mix formation electrolytic solution, TETRADECONIC ACID powder add-on is 0.08mol/L～0.5mol/L;
Step 3: in electrolytic solution, put into two copper sheets as anode and negative electrode, the volts DS that between anode and negative electrode, loads 15～30V carries out electrolysis, and electrolysis time is 10min～30min;
Step 4: after electrolysis is accomplished, anode and negative electrode are cleaned in zero(ppm) water afterwards in drying at room temperature, obtain the TETRADECONIC ACID copper film of micro, obtain being inlaid with the TETRADECONIC ACID iron thin film of ferric oxide particles at negative electrode at anode.
2. the method for utilizing iron(ic)chloride to prepare two kinds of based superhydrophobic thin films simultaneously according to claim 1 is characterized in that:
Described two copper sheet size 60mm * 25mm * 1.5mm.
3. the method for utilizing iron(ic)chloride to prepare two kinds of based superhydrophobic thin films simultaneously according to claim 1 and 2 is characterized in that: the contact angle of negative electrode and anode copper sheet all is transformed into super-hydrophobicity from wetting ability and reaches 160 °, and roll angle is less than 2 °.
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| CN102345148B (en) * | 2011-07-28 | 2013-12-25 | 西北工业大学 | Method for rapidly preparing cathode super-hydrophobic surface coatings containing rare earth elements through electrodeposition |
| CN102352499A (en) * | 2011-09-08 | 2012-02-15 | 西北工业大学 | Method for preparing metal carboxylate super-hydrophobic coating on surface of metal |
| CN105297082A (en) * | 2015-11-05 | 2016-02-03 | 华南理工大学 | Method for preparing super-hydrophobic film layers on metal surfaces through one-step method |
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Non-Patent Citations (3)
| Title |
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| Shutao Wang et al..One-Step Solution-Immersion Process for the Fabrication of Stable Bionic Superhydrophobic Surfaces.《Advanced Materials》.2006,第18卷767-770. * |
| Tao Liu et al..Corrosion behavior of super-hydrophobic surface on copper in seawater.《Electrochimica Acta 》.2007,第52卷8003-8007. * |
| 赵宁 等.超疏水表面的研究进展.《化学进展》.2007,第19卷(第6期),860-871. * |
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