CN103320827B - A kind of preparation method of inorganic-salt-dopednano nano zinc oxide film - Google Patents
A kind of preparation method of inorganic-salt-dopednano nano zinc oxide film Download PDFInfo
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- CN103320827B CN103320827B CN201310233266.6A CN201310233266A CN103320827B CN 103320827 B CN103320827 B CN 103320827B CN 201310233266 A CN201310233266 A CN 201310233266A CN 103320827 B CN103320827 B CN 103320827B
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Abstract
The present invention relates to a kind of preparation method of inorganic-salt-dopednano nano zinc oxide film, specifically comprise following step poly-: first configure precursor solution, zinc source is zinc nitrate or zinc chloride, and inorganic salt are sodium-chlor or SODIUMNITRATE, drips a certain amount of inorganic salt in zinc solution; Then first body solution is proceeded to three-electrode system, wherein using conductive substrates as working electrode, platinum electrode as supporting electrode, saturated calomel electrode as reference electrode, depositing temperature 25-50 DEG C, depositing time 5-20min, sedimentation potential-0.9V ~-1.5V; Finally carry out aftertreatment, by product rinsing, drying, 500 DEG C of calcining 1h.The inventive method is simple to operate, and cost is low, and the product of preparation is white, hexagonal system Pb-Zn deposits structure.
Description
Technical field
The invention belongs to nano semiconductor material preparing technical field, relate to the preparation method of Nano zinc oxide film, particularly a kind of electrochemical deposition method prepares the method for inorganic salt blended depositing nano zinc-oxide film.
Background technology
Along with the needs of the progress of science and technology, the development of production practice and Military Application, people need to manufacture the important materials of blue ultraviolet laser and detector and radioprotective, high temperature, HIGH-POWERED MICROWAVES electron device, the demand of all societies has evoked the research interest of people to semiconductor material, in third generation semiconductor material, owing to manufacturing the high cost of GaN material and expensive equipment, people wish to find the substitute products close with GaN character.
In recent years, zinc oxide is as a kind of important broad stopband direct band-gap semicondictor material, cause people more and more to pay attention to, it is easy to realize high efficiency Laser emission under room temperature or higher temperature, significantly can reduce threshold current, and the Zinc oxide-base device making manufacturing price cheap becomes possibility, is easy to make small size device.It is transparent in very large wavelength region that the character of zinc oxide material determines zinc oxide, has low-k and good photoelectricity and piezoelectric property, in solar cell, detector, optical waveguides etc., have very large application potential.
The method preparing zinc oxide has a variety of, and electrochemical deposition method can carry out at normal temperatures and pressures, and technique is simple, and easy to operate, cost is low, environmentally friendly, preparing the advantage in film nano material with uniqueness, is more and more subject to people's attention.In electrochemical deposition process, in order to the electromigration of eliminative reaction thing, usually add inorganic salt in the electrolytic solution as supporting electrolyte, improve the electroconductibility of solution, electrochemical deposition process is stablized more smoothly and carries out.
Summary of the invention
Technical scheme of the present invention is as follows: a kind of preparation method of inorganic-salt-dopednano nano zinc oxide film, first preparation is containing the precursor solution of zinc, then mix inorganic salt and be made into electrolytic solution, carry out electrochemical deposition subsequently, finally namely settling anneal is obtained Nano zinc oxide film.
In a more excellent disclosed example of the present invention, the step of preparation electrolytic solution is in 50ml zinc solution, add inorganic salt under room temperature, and place stand-by after stirring, described zinc salt and the mol ratio of inorganic salt are (0.05-0.1): (0.05-0.1).Place stand-by after stirring, the volumetric molar concentration of described zinc solution is 0.05 ~ 0.1molL
-1, described inorganic salt concentration is 0.05-0.1molL
-1.
In a more excellent disclosed example of the present invention, described electrochemical deposition is proceeded in three-electrode system by above-mentioned precursor solution to deposit, wherein, described three-electrode system is using conductive substrates as working electrode, platinum electrode as supporting electrode, saturated calomel electrode as reference electrode, depositing temperature 25 ~ 50 DEG C, depositing time 5 ~ 20min, sedimentation potential-0.9 ~-1.5V.
In a more excellent disclosed example of the present invention, described post-processing step is by through the product deionized water rinsing of electrochemical deposition gained, drying, is placed in retort furnace in 500 DEG C of calcining 1h, is cooled to room temperature.
In a more excellent disclosed example of the present invention, described conductive substrates is ITO conductive glass, and described sedimentation potential is-1.1V, the preferred 10min of depositing time preferably.
In a more excellent disclosed example of the present invention, described zinc salt is any one in zinc nitrate, zinc chloride.
In a more excellent disclosed example of the present invention, described inorganic salt are the one in sodium-chlor, SODIUMNITRATE.
Nano zinc oxide film prepared by method disclosed by the invention is hexagonal wurtzite structure.
The present invention's reagent zinc nitrate, zinc chloride, sodium-chlor and SODIUMNITRATE used is analytical pure.
beneficial effect
The present invention prepares inorganic salt blended depositing nano zinc-oxide film by electrochemical deposition method, improves the stability of thin film deposition, the present invention have be easy to control, cost is low, the advantage of technique and simple flow, be applicable to suitability for industrialized production.
Accompanying drawing explanation
The Electron micrographs figure (SEM) of Fig. 1 embodiment 1
The Electron micrographs figure (SEM) of Fig. 2 embodiment 5
The XRD figure of Fig. 3 embodiment 1.
Embodiment
embodiment 1
1, prepare precursor solution 50ml, zinc source is zinc nitrate (1.487g), and inorganic salt are sodium-chlor (0.2922g), zinc nitrate 0.1molL in electrolytic solution
-1, sodium chloride concentration 0.1molL
-1.
2, carry out electrochemical deposition, precursor solution is proceeded to three-electrode system, wherein using ITO conductive glass as working electrode, platinum electrode as supporting electrode, saturated calomel electrode as reference electrode, depositing temperature 25 DEG C, depositing time 10min, sedimentation potential-1.1V;
3, aftertreatment, by product deionized water rinsing, drying repeatedly, 500 DEG C of calcining 1h, obtain Nano zinc oxide film, product is polycrystalline hexagonal wurtzite structure, and Electron micrographs figure (SEM) is shown in Fig. 1, and XRD is as Fig. 3.
embodiment 2
1, prepare precursor solution 50ml, zinc source is zinc nitrate (1.487g), and inorganic salt are SODIUMNITRATE (0.425g), and in electrolytic solution, zinc nitrate and sodium nitrate concentration are all 0.1molL
-1.
2, carry out electrochemical deposition, precursor solution is proceeded to three-electrode system, wherein using ITO conductive glass as working electrode, platinum electrode as supporting electrode, saturated calomel electrode as reference electrode, depositing temperature 50 DEG C, depositing time 5min, sedimentation potential-1.1V;
3, aftertreatment, by product deionized water rinsing, drying repeatedly, 500 DEG C of calcining 1h, obtain Nano zinc oxide film, product is polycrystalline hexagonal wurtzite structure.
embodiment 3
1, prepare precursor solution 50ml, zinc source is zinc chloride (0.34g), and inorganic salt are sodium-chlor (0.146g), zinc oxide concentration 0.05molL in electrolytic solution
-1, sodium chloride concentration 0.05molL
-1.
2, carry out electrochemical deposition, precursor solution is proceeded to three-electrode system, wherein using ITO conductive glass as working electrode, platinum electrode as supporting electrode, saturated calomel electrode as reference electrode, depositing temperature 25 DEG C, depositing time 5min, sedimentation potential-0.9V;
3, aftertreatment, by product deionized water rinsing, drying repeatedly, 500 DEG C of calcining 1h, obtain Nano zinc oxide film, product is polycrystalline hexagonal wurtzite structure.
embodiment 4
1, prepare precursor solution 50ml, zinc source is zinc chloride (0.68g), and inorganic salt are SODIUMNITRATE (0.425g), and in electrolytic solution, zinc chloride and sodium nitrate concentration are all 0.1molL
-1.
2, carry out electrochemical deposition, precursor solution is proceeded to three-electrode system, wherein using ITO conductive glass as working electrode, platinum electrode as supporting electrode, saturated calomel electrode as reference electrode, depositing temperature 25 DEG C, depositing time 20min, sedimentation potential-1.5V;
3, aftertreatment, by product deionized water rinsing, drying repeatedly, 500 DEG C of calcining 1h, obtain Nano zinc oxide film, product is polycrystalline hexagonal wurtzite structure.
embodiment 5
1, prepare precursor solution 50ml, zinc source is zinc nitrate (1.487g), and inorganic salt are SODIUMNITRATE (0.425g), and in electrolytic solution, zinc nitrate and sodium nitrate concentration are all 0.1molL
-1.
2, carry out electrochemical deposition, precursor solution is proceeded to three-electrode system, wherein using ITO conductive glass as working electrode, platinum electrode as supporting electrode, saturated calomel electrode as reference electrode, depositing temperature 25 DEG C, depositing time 10min, sedimentation potential-1.1V;
3, aftertreatment, by product deionized water rinsing, drying repeatedly, 500 DEG C of calcining 1h, obtain Nano zinc oxide film, product is polycrystalline hexagonal wurtzite structure, and Electron micrographs figure (SEM) is shown in Fig. 2.
Claims (4)
1. the preparation method of an inorganic-salt-dopednano nano zinc oxide film, carry out according to following step: first preparation is containing the precursor solution of zinc, then mix inorganic salt and be made into electrolytic solution, carry out electrochemical deposition subsequently, finally namely settling anneal is obtained Nano zinc oxide film;
The step wherein preparing electrolytic solution is, in 50ml zinc solution, inorganic salt are added under room temperature, place stand-by after stirring, described zinc salt and the mol ratio of inorganic salt are (0.05-0.1): (0.05-0.1), and the volumetric molar concentration of described zinc solution is 0.05 ~ 0.1molL
-1, described inorganic salt concentration is 0.05-0.1molL
-1;
Wherein said electrochemical deposition is proceeded in three-electrode system by above-mentioned electrolytic solution to deposit, wherein said three-electrode system is using conductive substrates as working electrode, platinum electrode is as supporting electrode, saturated calomel electrode is as reference electrode, depositing temperature 25 ~ 50 DEG C, depositing time 5 ~ 20min, sedimentation potential-0.9 ~-1.5V;
Be wherein by through the product deionized water rinsing of electrochemical deposition gained, drying by settling anneal, be placed in retort furnace in 500 DEG C of calcining 1h, be cooled to room temperature.
2. the preparation method of inorganic-salt-dopednano nano zinc oxide film according to claim 1, is characterized in that: described conductive substrates is ITO conductive glass, and described sedimentation potential is-1.1V, and depositing time is 10min.
3. the preparation method of inorganic-salt-dopednano nano zinc oxide film according to claim 1, is characterized in that: described zinc salt is zinc nitrate or zinc chloride.
4. the preparation method of inorganic-salt-dopednano nano zinc oxide film according to claim 1, is characterized in that: described inorganic salt are sodium-chlor or SODIUMNITRATE.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101348931A (en) * | 2008-09-11 | 2009-01-21 | 北京科技大学 | Method for preparing uniform transparent zinc oxide nanorod array film by pulse electrodeposition |
| CN103060873A (en) * | 2013-01-17 | 2013-04-24 | 河南科技大学 | Method for preparing porous array ZnO thin film in graded structure by electro-deposition method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101348931A (en) * | 2008-09-11 | 2009-01-21 | 北京科技大学 | Method for preparing uniform transparent zinc oxide nanorod array film by pulse electrodeposition |
| CN103060873A (en) * | 2013-01-17 | 2013-04-24 | 河南科技大学 | Method for preparing porous array ZnO thin film in graded structure by electro-deposition method |
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