CN104018200A - Method for enhancing surface wettability of hexagonal-prism-structure nano zinc oxide material - Google Patents
Method for enhancing surface wettability of hexagonal-prism-structure nano zinc oxide material Download PDFInfo
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Abstract
The invention discloses a method for enhancing surface wettability of a hexagonal-prism-structure nano zinc oxide material, relating to a method for lowering surface energy of zinc oxide. The surface contact angle and roll angle of the fluorizated hexagonal-prism-structure nano zinc oxide are enhanced, and the Cu2O/ZnO composite material can enhance the photoelectric conversion efficiency. The method adopts an electrochemical deposition process and comprises the following steps: by using copper sulfate, lactic acid and sodium hydroxide as raw materials, adding cationic and nonionic surfactants; in a two-electrode system, by using graphite as an anode and an ITO (indium tin oxide) glass sheet deposited with hexagonal-prism-structure zinc oxide structure as a cathode, carrying out cathode reduction while controlling the deposition voltage, time and temperature to deposit granular cuprous oxide on the hexagonal-prism-structure zinc oxide, sintering at certain temperature, treating with a low-surface-energy substance, and measuring the surface static contact angle. The method has the advantages of low production cost, simple preparation process, low requirements for reaction equipment, mild reaction conditions and no environmental pollution, and can large-scale production.
Description
Technical field
The present invention relates to a kind of method that improves hexa-prism structure nano zinc oxide material surface wettability.
Background technology
Zinc oxide is a kind of N-type semiconductor material with direct band gap, energy gap 3.37 eV, and theoretical lithium amount 978 mAh/g of place, at photoelectricity, photochemical catalysis, dye sensitized nano crystal salar battery, the field extensive application such as lithium ion battery.Hexa-prism zinc oxide, after silicon fluoride is processed, show as superhydrophobic characteristic, but its surperficial static contact angle is 152
oleft and right, roll angle is greater than 7
o.Cu
2the 0th, a kind of typical P-type semiconductor material, energy gap is 2.1 eV, can be 10 according to the different resistivity of preparation condition
3～10
13within the scope of Ω cm, change.The suction of visible-range, receives coefficient higher, and energy transformation ratio can reach 10% in theory, has lower surface energy and energy gap and better catalytic activity with respect to ZnO.At present, the Wei Hao of University Of Ji'nan inscription waits zinc oxide/cuprous oxide (ZnO/Cu
2o) two kinds of typical n/p semi-conductors are research object, and its opto-electronic conversion performance is studied.But, the impact of ZnO wettability of the surface is not done to correlative study.Therefore,, at hexa-prism nano zinc oxide material surface electrical deposited particles shape Red copper oxide, through fluoridation, its surface wettability can obviously improve.
Summary of the invention
In order to improve hexa-prism ZnO nano material wettability of the surface energy, the invention provides a kind of method of the wettability that improves hexa-prism structure nano ZnO material surface.
The technical solution used in the present invention is: taking the ito glass sheet that deposits hexa-prism nano zine oxide as substrate, taking copper sulfate, lactic acid, sodium hydroxide as raw material, add positively charged ion and nonionogenic tenside, in two electrode systems, control deposition voltage, time-temperature, through cathodic reduction deposited particles shape Red copper oxide on hexa-prism zinc oxide, after certain temperature sintering, by low surface energy mass treatment and measure its surface static contact angle.
It is of the present invention that to prepare feature process step as follows:
One, compound concentration is the copper sulfate solution of 0.005 ~ 0.1 mol/L, adds positively charged ion or nonionic surface active agent in solution, and both mol ratios are 1:1 ~ 1:5;
Two, using the pH value of lactic acid, sodium hydrate regulator solution is 9 ~ 12;
Three, use two electrode systems, wherein Graphite Electrodes is anode, and the ito glass sheet of 1.5 cm*5 cm is negative electrode, at constant voltage 2.5 V, under the condition that constant temperature is 50 ~ 70 DEG C, carries out electrochemical deposition, and depositing time is 10 s ~ 5 min;
Four, galvanic deposit is obtained to the long ito glass plate electrode that has Red copper oxide, anneal 1 ~ 4 h in the sintering oven of 300 ~ 500 DEG C, obtains the long Red copper oxide that has ad hoc structure on six prism zinc oxide;
Five,, by the ITO electrode after galvanic deposit, putting into volume ratio is that the perfluoro capryl triethoxyl silane of 1:1000 ~ 1:200 or the ethanolic soln of Dodecyl Mercaptan soak 1 h ~ 48 h;
Six, take out the ITO electrode after soaking, survey the static contact angle of surface of nanometer zinc oxide with contact angle measurement, obtain its surface contact angle 158
o~ 173
o, roll angle is 2
o~ 7
o, result shows to have improved its surface wettability after pillar shaped ZnO substrates Red copper oxide.
Further, the cationic surfactant adding in the aqueous solution in described step 1 is quaternary, and nonionic surface active agent is arlacels.
Further, in described step 1, the volumetric molar concentration of cats product is 0.05 ~ 10 mmol/L.
Further, in described step 4, annealing is to carry out in air, does not contain other protective gas.
Advantage of the present invention is: (1) is fine granularity at the Red copper oxide of hexa-prism zinc oxide surface galvanic deposit, is evenly distributed at zinc oxide surface, and through silicon fluoride and Dodecyl Mercaptan processing, its surperficial contact angle increases greatly, and roll angle is corresponding to be reduced; (2) present method can be grown directly upon on electrode, and its sticking power is more much better than general coating process; (3) copper sulfate, lactic acid, sodium hydroxide and the tensio-active agents etc. that the present invention uses are all conventional raw materials, and production cost is low, low to conversion unit requirement, reaction conditions gentleness, and preparation method is simple, non-environmental-pollution.
Brief description of the drawings
Fig. 1 is the field emission scanning electron microscope figure of hexa-prism structure nano zinc oxide substrates Red copper oxide of the present invention.
Fig. 2 is the EDS figure of hexa-prism structure nano zinc oxide substrates Red copper oxide of the present invention.
Fig. 3 be hexa-prism structure nano zinc oxide substrates of the present invention Red copper oxide through silicon fluoride modify after static contact angle schematic diagram.
Fig. 4 is Red copper oxide roll angle schematic diagram after silicon fluoride is modified of hexa-prism structure nano zinc oxide substrates of the present invention.
Embodiment
Provides embodiments of the invention and in conjunction with the embodiment providing, the present invention be illustrated, but given embodiment does not constitute any limitation the present invention:
Embodiment one: compound concentration is the copper-bath of 0.005 mol/L, with the pH value of 1.5 mL lactic acid, sodium hydrate regulator solution be 11; In two electrode systems, wherein Graphite Electrodes is anode, and the ito glass sheet of 1.5 cm*5 cm is negative electrode, at constant voltage 2.5 V, under the condition that constant temperature is 50 DEG C, carries out electrochemical deposition, and depositing time is 10s; The length that galvanic deposit is obtained has the ito glass plate electrode of zinc oxide, anneal 4 hours in the sintering oven of 400 DEG C, obtain the long Red copper oxide that has ad hoc structure on six prism zinc oxide, by the ITO electrode after galvanic deposit, the ethanolic soln of putting into volume ratio and be the perfluoro capryl triethoxyl silane of 1:1000 soaks 24 h; Take out the ITO electrode after soaking, survey static contact angle and the roll angle of surface of nanometer zinc oxide with contact angle measurement, obtain more excellent superhydrophobic characteristic.
Embodiment two: compound concentration is the copper-bath of 0.005 mol/L, with the pH value of 1.5 mL lactic acid, sodium hydrate regulator solution be 10; In two electrode systems, wherein Graphite Electrodes is anode, and the ito glass sheet of 1.5 cm*5 cm is negative electrode, at constant voltage 2.5 V, under the condition that constant temperature is 50 DEG C, carries out electrochemical deposition, and depositing time is 30 s; Galvanic deposit is obtained to the long ito glass plate electrode that has Red copper oxide, anneal 4 h in the sintering oven of 400 DEG C, obtain the long Red copper oxide that has ad hoc structure on six prism zinc oxide, by the ITO electrode after galvanic deposit, the ethanolic soln of putting into volume ratio and be the perfluoro capryl triethoxyl silane of 1:1000 soaks 24 h; Take out the ITO electrode after soaking, survey static contact angle and the roll angle of surface of nanometer zinc oxide with contact angle measurement, obtain more excellent superhydrophobic characteristic.
Embodiment three: compound concentration is the copper-bath of 0.005 mol/L, with the pH value of 1.5 mL lactic acid, sodium hydrate regulator solution be 9; In solution, add the cationicsurfactants of 3 mmol/L, in two electrode systems, wherein Graphite Electrodes is anode, the ito glass sheet of 1.5 cm*5 cm is negative electrode, at constant voltage 2.5 V, under the condition that constant temperature is 50 DEG C, carry out electrochemical deposition, depositing time is 5 min; Galvanic deposit is obtained to the long ito glass plate electrode that has Red copper oxide, anneal 5 h in the sintering oven of 400 DEG C, obtain the long Red copper oxide that has ad hoc structure on six prism zinc oxide, by the ITO electrode after galvanic deposit, the ethanolic soln of putting into volume ratio and be the Dodecyl Mercaptan of 1:1000 soaks 2h; Take out the ITO electrode after soaking, survey static contact angle and the roll angle of surface of nanometer zinc oxide with contact angle measurement, obtain more excellent characteristic.
Embodiment four: compound concentration is the copper-bath of 0.005 mol/L, with the pH value of 1.5 mL lactic acid, sodium hydrate regulator solution be 12; In two electrode systems, wherein Graphite Electrodes is anode, and the ito glass sheet of 1.5 cm*5 cm is negative electrode, at constant voltage 2.5 V, under the condition that constant temperature is 50 DEG C, carries out electrochemical deposition, and depositing time is 5 min; Galvanic deposit is obtained to the long ito glass plate electrode that has Red copper oxide, anneal 4 h in the sintering oven of 400 DEG C, obtain the long Red copper oxide that has ad hoc structure on six prism zinc oxide, by the ITO electrode after galvanic deposit, the ethanolic soln of putting into volume ratio and be the Dodecyl Mercaptan of 1:1000 soaks 4 h; Take out the ITO electrode after soaking, survey static contact angle and the roll angle of surface of nanometer zinc oxide with contact angle measurement, obtain more excellent characteristic.
Embodiment five: compound concentration is the copper-bath of 0.05 mol/L, with the pH value of 1.5 mL lactic acid, sodium hydrate regulator solution be 10; In two electrode systems, wherein Graphite Electrodes is anode, and the ito glass sheet of 1.5 cm*5 cm is negative electrode, at constant voltage 2.5 V, under the condition that constant temperature is 50 DEG C, carries out electrochemical deposition, and depositing time is 20 s; Galvanic deposit is obtained to the long ito glass plate electrode that has Red copper oxide, anneal 4 hours in the sintering oven of 400 DEG C, obtain the long Red copper oxide that has ad hoc structure on six prism zinc oxide, by the ITO electrode after galvanic deposit, put into volume ratio and be 1:1000 perfluoro capryl triethoxyl silane ethanolic soln soak 12 h; Take out the ITO electrode after soaking, survey static contact angle and the roll angle of surface of nanometer zinc oxide with contact angle measurement, obtain more excellent characteristic.
Embodiment six: compound concentration is the copper-bath of 0.05 mol/L, with the pH value of 1.5 mL lactic acid, sodium hydrate regulator solution be 11; In solution, add nonionic surface active agent polyoxyethylene glycol, in two electrode systems, wherein Graphite Electrodes is anode, the ito glass sheet of 1.5 cm*5 cm is negative electrode, at constant voltage 2.5 V, under the condition that constant temperature is 50 DEG C, carry out electrochemical deposition, depositing time is 1 min; Galvanic deposit is obtained to the long ito glass plate electrode that has Red copper oxide, anneal 4 hours in the sintering oven of 400 DEG C, obtain the long Red copper oxide that has ad hoc structure on six prism zinc oxide, by the ITO electrode after galvanic deposit, the ethanolic soln of putting into volume ratio and be the perfluoro capryl triethoxyl silane of 1:1000 soaks 24 h; Take out the ITO electrode after soaking, survey static contact angle and the roll angle of surface of nanometer zinc oxide with contact angle measurement, obtain more excellent superhydrophobic characteristic.
Embodiment seven: compound concentration is the copper-bath of 0.05 mol/L, with the pH value of 1.5 mL lactic acid, sodium hydrate regulator solution be 11; In two electrode systems, wherein Graphite Electrodes is anode, and the ito glass sheet of 1.5 cm*5 cm is negative electrode, at constant voltage 2.5 V, under the condition that constant temperature is 50 DEG C, carries out electrochemical deposition, and depositing time is 10 s; Galvanic deposit is obtained to the long ito glass plate electrode that has Red copper oxide, anneal 3 h in the sintering oven of 400 DEG C, obtain the long Red copper oxide that has ad hoc structure on six prism zinc oxide, by the ITO electrode after galvanic deposit, the ethanolic soln of putting into volume ratio and be the perfluoro capryl triethoxyl silane of 1:1000 soaks 24 h; Take out the ITO electrode after soaking, survey static contact angle and the roll angle of surface of nanometer zinc oxide with contact angle measurement, obtain more excellent superhydrophobic characteristic.
Embodiment eight: compound concentration is the copper-bath of 0.05 mol/L, with the pH value of 1.5 mL lactic acid, sodium hydrate regulator solution be 10; In two electrode systems, wherein Graphite Electrodes is anode, and the ito glass sheet of 1.5 cm*5 cm is negative electrode, at constant voltage 2.5 V, under the condition that constant temperature is 50 DEG C, carries out electrochemical deposition, and depositing time is 30 s; Galvanic deposit is obtained to the long ito glass plate electrode that has Red copper oxide, anneal 4 hours in the sintering oven of 400 DEG C, obtain the long Red copper oxide that has ad hoc structure on six prism zinc oxide, by the ITO electrode after galvanic deposit, the ethanolic soln of putting into volume ratio and be the perfluoro capryl triethoxyl silane of 1:1000 soaks 24h; Take out the ITO electrode after soaking, survey static contact angle and the roll angle of surface of nanometer zinc oxide with contact angle measurement, obtain more excellent superhydrophobic characteristic.
Embodiment nine: compound concentration is the copper-bath of 0.05 mol/L, with the pH value of 1.5 mL lactic acid, sodium hydrate regulator solution be 9; In two electrode systems, wherein Graphite Electrodes is anode, and the ito glass sheet of 1.5 cm*5 cm is negative electrode, at constant voltage 2.5 V, under the condition that constant temperature is 50 DEG C, carries out electrochemical deposition, and depositing time is 1 min; Galvanic deposit is obtained to the long ito glass plate electrode that has Red copper oxide, anneal 4 h in the sintering oven of 400 DEG C, obtain the long Red copper oxide that has ad hoc structure on six prism zinc oxide, by the ITO electrode after galvanic deposit, the ethanolic soln of putting into volume ratio and be the perfluoro capryl triethoxyl silane of 1:1000 soaks 24 h; Take out the ITO electrode after soaking, survey static contact angle and the roll angle of surface of nanometer zinc oxide with contact angle measurement, obtain more excellent superhydrophobic characteristic.
Embodiment ten: compound concentration is the copper-bath of 0.1 mol/L, with the pH value of 1.5 mL lactic acid, sodium hydrate regulator solution be 9; In two electrode systems, wherein Graphite Electrodes is anode, and the ito glass sheet of 1.5 cm*5 cm is negative electrode, at constant voltage 2.5 V, under the condition that constant temperature is 60 DEG C, carries out electrochemical deposition, and depositing time is 10 s; Galvanic deposit is obtained to the long ito glass plate electrode that has Red copper oxide, anneal 4 h in the sintering oven of 400 DEG C, obtain the long Red copper oxide that has ad hoc structure on six prism zinc oxide, by the ITO electrode after galvanic deposit, the ethanolic soln of putting into volume ratio and be the perfluoro capryl triethoxyl silane of 1:1000 soaks 24 h; Take out the ITO electrode after soaking, survey static contact angle and the roll angle of surface of nanometer zinc oxide with contact angle measurement, obtain more excellent superhydrophobic characteristic.
Embodiment 11: compound concentration is the copper-bath of 0.1 mol/L, with the pH value of 1.5 mL lactic acid, sodium hydrate regulator solution be 11; In two electrode systems, wherein Graphite Electrodes is anode, and the ito glass sheet of 1.5 cm*5 cm is negative electrode, at constant voltage 2.5 V, under the condition that constant temperature is 70 DEG C, carries out electrochemical deposition, and depositing time is 1 min; Galvanic deposit is obtained to the long ito glass plate electrode that has Red copper oxide, anneal 4 h in the sintering oven of 400 DEG C, obtain the long Red copper oxide that has ad hoc structure on six prism zinc oxide, by the ITO electrode after galvanic deposit, the ethanolic soln of putting into volume ratio and be the Dodecyl Mercaptan of 1:500 soaks 4 h; Take out the ITO electrode after soaking, survey static contact angle and the roll angle of surface of nanometer zinc oxide with contact angle measurement, obtain more excellent superhydrophobic characteristic.
Claims (4)
1. a method that improves hexa-prism structure nano zinc oxide material surface wettability, is characterized in that: have the relatively Red copper oxide of low surface energy at the zinc oxide substrates of hexa-prism structure, carry out according to the following steps:
One, compound concentration is the copper sulfate solution of 0.005 ~ 0.1 mol/L, adds positively charged ion or nonionic surface active agent in solution;
Two, using the pH value of lactic acid, sodium hydrate regulator solution is 9 ~ 12;
Three, use two electrode systems, wherein Graphite Electrodes is anode, and the ito glass sheet of 1.5 cm*5 cm is negative electrode, at constant voltage 2.5 V, under the condition that constant temperature is 50 ~ 70 DEG C, carries out electrochemical deposition, and depositing time is 10 s ~ 5 min;
Four, galvanic deposit is obtained to the long ito glass plate electrode that has Red copper oxide, anneal 1 ~ 4 h in the sintering oven of 300 ~ 500 DEG C, obtains the long Red copper oxide that has ad hoc structure on six prism zinc oxide;
Five,, by the ITO electrode after galvanic deposit, putting into volume ratio is that the perfluoro capryl triethoxyl silane of 1:1000 ~ 1:200 or the ethanolic soln of Dodecyl Mercaptan soak 1 h ~ 48 h;
Six, take out the ITO electrode after soaking, survey the static contact angle of surface of nanometer zinc oxide with contact angle measurement, obtaining its surface contact angle is 158
o~ 173
o, roll angle is 2
o~ 7
o, result shows to have improved its surface wettability after pillar shaped ZnO substrates Red copper oxide.
2. a kind of method that improves hexa-prism structure nano zinc oxide material surface wettability according to claim 1, it is characterized in that: the cationic surfactant adding in the aqueous solution in described step 1 is quaternary, nonionic surface active agent is arlacels.
3. a kind of method that improves hexa-prism structure nano zinc oxide material surface wettability according to claim 1, it is characterized in that: in step 1, the mol ratio of positively charged ion and nonionic surface active agent is 1:1 ~ 1:5, wherein the volumetric molar concentration of cats product is 0.05 ~ 10 mmol/L.
4. a kind of method that improves hexa-prism structure nano zinc oxide material surface wettability according to claim 1, is characterized in that: in step 4, annealing is to carry out in air, does not contain other protective gas.
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Cited By (3)
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| CN107694866A (en) * | 2017-11-10 | 2018-02-16 | 中国第汽车集团公司新能源汽车分公司 | A kind of method of oxide nanofiber auxiliary stator winding dipping lacquer |
| CN108611630A (en) * | 2018-04-11 | 2018-10-02 | 燕山大学 | A kind of hierarchical Z nO/Cu3(PO4)2Controllable immersing composite material and preparation method |
| CN112748162A (en) * | 2021-01-28 | 2021-05-04 | 福州大学 | Ni/ZnO/Cu composite material electrode, preparation method and application thereof, and detection method of chemical oxygen demand of water body |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107694866A (en) * | 2017-11-10 | 2018-02-16 | 中国第汽车集团公司新能源汽车分公司 | A kind of method of oxide nanofiber auxiliary stator winding dipping lacquer |
| CN108611630A (en) * | 2018-04-11 | 2018-10-02 | 燕山大学 | A kind of hierarchical Z nO/Cu3(PO4)2Controllable immersing composite material and preparation method |
| CN112748162A (en) * | 2021-01-28 | 2021-05-04 | 福州大学 | Ni/ZnO/Cu composite material electrode, preparation method and application thereof, and detection method of chemical oxygen demand of water body |
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