CN102229438B - Interface preparation method of flaky zinc oxide - Google Patents
Interface preparation method of flaky zinc oxide Download PDFInfo
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- CN102229438B CN102229438B CN 201110146200 CN201110146200A CN102229438B CN 102229438 B CN102229438 B CN 102229438B CN 201110146200 CN201110146200 CN 201110146200 CN 201110146200 A CN201110146200 A CN 201110146200A CN 102229438 B CN102229438 B CN 102229438B
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Abstract
The invention discloses an interface preparation method of flaky zinc oxide. The method comprises the following steps: 1) adding excessive ammonia water in a water solution of zinc salt, and then adding an accelerating agent to obtain a clear solution; 2) exposing the clear solution obtained in the step 1) to the air and standing for forming a membrane on the surface of the solution; and 3) taking the membrane formed in the step 2) out, washing and calcining to finally obtain the flaky zinc oxide. The technology method provided by the invention is simple, environmentally-friendly and pollution-free, is convenient to operate, has moderate reaction conditions, and does not need special devices.
Description
Technical field
The present invention relates to a kind of interface preparation method of sheet zinc oxide.
Background technology
ZnO is as a kind of broad-band gap, the n-type semiconductor oxide of high excitation energy has many good character. and the sheet zinc oxide with certain pattern has unique piezo-electricity, high specific conductivity, photocatalysis and scattering and the ability of absorbing ultraviolet, can be applied to varistor, sensor, many fields such as photochemical catalysis.
The method of tradition making ZnO mainly comprises vapour deposition and chemosynthesis (hydrothermal method, sol-gel method, the precipitator method etc.), these synthetic methods need to realize under high temperature or the hyperbaric environment and in other specific installation situations mostly, belong to the synthetic category of thermochemistry.Exist to a certain extent production cost height, severe reaction conditions, technique and be difficult to the problems such as control, complex manufacturing, for this reason, be necessary to develop the simply synthetic ZnO semiconductor material of a kind of low cost, high-level efficiency.
Summary of the invention
The interface preparation method that the purpose of this invention is to provide a kind of sheet zinc oxide.
The technical solution used in the present invention is:
A kind of interface preparation method of sheet zinc oxide may further comprise the steps:
1) in the aqueous solution of zinc salt, adds excess of ammonia water, add again promotor, obtain clear soln;
2) settled solution that step 1) is obtained is exposed in the air and leaves standstill, and forms film at liquid level;
3) take out step 2) the middle film that forms, washing, calcining gets sheet zinc oxide.
Zinc salt is 1:1-2 with the ratio of the amount of substance of promotor.
Described zinc salt is a kind of in zinc sulfate, zinc chloride, the zinc nitrate.
Described promotor is the salt of alkalescence for hydrolysis.
The temperature of calcining is 400-600 ℃.
The time of calcining is 2-6h.
The invention has the beneficial effects as follows: processing method of the present invention is simple, and reaction conditions is gentle, and environmentally friendly, green non-pollution need not special device, and is simple to operate, the products obtained therefrom substantially free of impurities.
Description of drawings
Fig. 1 is the X-ray diffractogram of the sheet zinc oxide that makes of the embodiment of the invention 1;
Fig. 2 is the scanning electron microscope diagram sheet of the Zinc oxide film that makes of the embodiment of the invention 1;
Fig. 3 is the scanning electron microscope diagram sheet of the Zinc oxide film that makes of the embodiment of the invention 4;
Fig. 4 is the scanning electron microscope diagram sheet of the Zinc oxide film that makes of the embodiment of the invention 5;
Fig. 5 is the scanning electron microscope diagram sheet of the Zinc oxide film that makes of the embodiment of the invention 6;
Fig. 6 is the scanning electron microscope diagram sheet of the Zinc oxide film that makes of the embodiment of the invention 8;
Fig. 7 is the scanning electron microscope diagram sheet of the Zinc oxide film that makes of the embodiment of the invention 9;
Fig. 8 is the scanning electron microscope diagram sheet of the Zinc oxide film that makes of the embodiment of the invention 10.
Embodiment
A kind of interface preparation method of sheet zinc oxide may further comprise the steps:
1) in the aqueous solution of zinc salt, adds excess of ammonia water, add again promotor, obtain clear soln; Wherein, zinc salt is 1:1-2 with the ratio of the amount of substance of promotor, solute (NH in zinc salt and the ammoniacal liquor
3H
2O) mol ratio is preferably 1:9-12.
2) settled solution that step 1) is obtained is exposed in the air and leaves standstill, and forms film at liquid level;
3) take out step 2) the middle film that forms, washing, calcining gets sheet zinc oxide.
The present invention is described further below in conjunction with specific embodiment:
Embodiment 1:
Taking by weighing 2.8756g Zinc vitriol and 2.52g sodium sulphite anhydrous 99.3 is dissolved in respectively in the deionized water of 100ml, dripping 8ml concentration in solution of zinc sulfate is the ammoniacal liquor of 12mol/L, make zine ion all be converted into zinc ammonia complex, then sodium sulfite solution is added in the zinc ammonia solution, be exposed at last 2h in the air, after reaction finishes, pick up upper layer film with slide, use deionized water wash 5-6 time, in baking oven, dry, place 400 ℃ of calcinings of retort furnace 2h, get sheet zinc oxide.
Embodiment 2:
Taking by weighing 2.8756g Zinc vitriol and 1.26g sodium sulphite anhydrous 99.3 is dissolved in respectively in the deionized water of 100ml, dripping 8ml concentration in solution of zinc sulfate is the ammoniacal liquor of 12mol/L, make zine ion all be converted into zinc ammonia complex, then sodium sulfite solution is added in the zinc ammonia solution, be exposed at last 4h in the air, after reaction finishes, pick up upper layer film with slide, use deionized water wash 5-6 time, in baking oven, dry, place retort furnace 400 degree calcining 2h, get sheet zinc oxide.
Embodiment 3:
Taking by weighing six methylene radical four ammonia of 2.8756g Zinc vitriol and 2.8g is dissolved in respectively in the deionized water of 100ml, dripping 10ml concentration in solution of zinc sulfate is the ammoniacal liquor of 12mol/L, make zine ion all be converted into zinc ammonia complex, then sodium sulfite solution is added in the zinc ammonia solution, be exposed at last 4h in the air, after reaction finishes, pick up upper layer film with slide, use deionized water wash 5-6 time, in baking oven, dry, place retort furnace 400 degree calcining 2h, get sheet zinc oxide.
Embodiment 4:
Taking by weighing 2.8756g Zinc vitriol and 2.52g sodium sulphite anhydrous 99.3 is dissolved in respectively in the deionized water of 100ml, dripping 8ml concentration in solution of zinc sulfate is the ammoniacal liquor of 12mol/L, make zine ion all be converted into zinc ammonia complex, then sodium sulfite solution is added in the zinc ammonia solution, place water-bath, 20 ℃ of constant temperature also are exposed to 2h in the air, after reaction finishes, pick up upper layer film with slide, with deionized water wash 5-6 time, in baking oven, dry, place retort furnace 400 degree calcining 2h, get sheet zinc oxide.
Embodiment 5:
Taking by weighing 2.8756g Zinc vitriol and 2.52g sodium sulphite anhydrous 99.3 is dissolved in respectively in the deionized water of 100ml, dripping 8ml concentration in solution of zinc sulfate is the ammoniacal liquor of 12mol/L, make zine ion all be converted into zinc ammonia complex, then sodium sulfite solution is added in the zinc ammonia solution, place water-bath, 30 ℃ of constant temperature also are exposed to 2h in the air, after reaction finishes, pick up upper layer film with slide, with deionized water wash 5-6 time, in baking oven, dry, place retort furnace 400 degree calcining 2h, get sheet zinc oxide.
Embodiment 6:
Taking by weighing 2.8756g Zinc vitriol and 2.52g sodium sulphite anhydrous 99.3 is dissolved in respectively in the deionized water of 100ml, dripping 8ml concentration in solution of zinc sulfate is the ammoniacal liquor of 12mol/L, make zine ion all be converted into zinc ammonia complex, then sodium sulfite solution is added in the zinc ammonia solution, place water-bath, 40 ℃ of constant temperature also are exposed to 2h in the air, after reaction finishes, pick up upper layer film with slide, with deionized water wash 5-6 time, in baking oven, dry, place retort furnace 400 degree calcining 2h, get sheet zinc oxide.
Embodiment 7:
Taking by weighing 2.8756g Zinc vitriol and 2.52g sodium sulphite anhydrous 99.3 is dissolved in respectively in the deionized water of 100ml, dripping 8ml concentration in solution of zinc sulfate is the ammoniacal liquor of 12mol/L, make zine ion all be converted into zinc ammonia complex, then sodium sulfite solution is added in the zinc ammonia solution, place water-bath, 50 ℃ of constant temperature also are exposed to 2h in the air, after reaction finishes, pick up upper layer film with slide, with deionized water wash 5-6 time, in baking oven, dry, place retort furnace 400 degree calcining 2h, get sheet zinc oxide.
Embodiment 8:
Taking by weighing 2.8756g zinc sulfate and 2.52g sodium sulphite anhydrous 99.3 is dissolved in respectively in the deionized water of 100ml, dripping 8ml concentration in solution of zinc sulfate is the ammoniacal liquor of 12mol/L, make zine ion all be converted into zinc ammonia complex, then sodium sulfite solution is added in the zinc ammonia solution, place water-bath, 60 ℃ of constant temperature also are exposed to 2h in the air, after reaction finishes, pick up upper layer film with slide, with deionized water wash 5-6 time, in baking oven, dry, place retort furnace 400 degree calcining 2h, get sheet zinc oxide.
Embodiment 9:
Taking by weighing 2.8756g zinc sulfate and 2.52g sodium sulphite anhydrous 99.3 is dissolved in respectively in the deionized water of 100ml, dripping 8ml concentration in solution of zinc sulfate is the ammoniacal liquor of 12mol/L, make zine ion all be converted into zinc ammonia complex, then sodium sulfite solution is added in the zinc ammonia solution, place water-bath, 70 ℃ of constant temperature also are exposed to 2h in the air, after reaction finishes, pick up upper layer film with slide, with deionized water wash 5-6 time, in baking oven, dry, place retort furnace 400 degree calcining 2h, get sheet zinc oxide.
Embodiment 9:
Taking by weighing 2.8756g zinc sulfate and 2.48g sodium sulphite anhydrous 99.3 is dissolved in respectively in the deionized water of 100ml, dripping 8ml concentration in solution of zinc sulfate is the ammoniacal liquor of 12mol/L, make zine ion all be converted into zinc ammonia complex, then sodium sulfite solution is added in the zinc ammonia solution, place water-bath, 70 ℃ of constant temperature also are exposed to 2h in the air, after reaction finishes, pick up upper layer film with slide, with deionized water wash 5-6 time, in baking oven, dry, place retort furnace 400 degree calcining 3h, get sheet zinc oxide.
Embodiment 10:
Taking by weighing 2.8756g zinc sulfate and 2.12g sodium sulphite anhydrous 99.3 is dissolved in respectively in the deionized water of 100ml, dripping 8ml concentration in solution of zinc sulfate is the ammoniacal liquor of 12mol/L, make zine ion all be converted into zinc ammonia complex, then sodium sulfite solution is added in the zinc ammonia solution, place water-bath, at room temperature and be exposed to 2h in the air, after reaction finishes, pick up upper layer film with slide, with deionized water wash 5-6 time, in baking oven, dry, place retort furnace 400 degree calcining 3h, get sheet zinc oxide.
Can find out from X-ray diffractogram, diffraction peak has clearly appearred in the ZnO of embodiment 1 preparation, 31.72 °, the crystal face (100) of 34.4 °, 36.2 °, 47.56 °, 56.64 °, the 62.94 ° corresponding ZnO of difference, (002), (101), (102), (110), (103), substantially free of impurities, can find out from Fig. 2-8, the ZnO pattern of the present invention's preparation is regular, and size distribution is even.
Claims (2)
1. the interface preparation method of a sheet zinc oxide is characterized in that: may further comprise the steps:
1) in the aqueous solution of zinc salt, adds excess of ammonia water, add again promotor, obtain clear soln;
2) settled solution that step 1) is obtained is exposed in the air and leaves standstill, and forms film at liquid level;
3) take out step 2) the middle film that forms, washing, calcining gets sheet zinc oxide;
Zinc salt is 1:1-2 with the ratio of the amount of substance of promotor; Described zinc salt is a kind of in zinc sulfate, zinc chloride, the zinc nitrate; Described promotor is the salt of alkalescence for hydrolysis; The temperature of calcining is 400-600 ℃.
2. the interface preparation method of a kind of sheet zinc oxide according to claim 1, it is characterized in that: the time of calcining is 2-6h.
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| CN 201110146200 CN102229438B (en) | 2011-06-01 | 2011-06-01 | Interface preparation method of flaky zinc oxide |
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| CN109956494B (en) * | 2017-12-22 | 2021-08-17 | 苏州大学 | Few-layer-structure ZnO two-dimensional nanosheet and preparation method thereof |
| DE102022111352A1 (en) | 2022-05-06 | 2023-11-09 | Leibniz-Institut für Photonische Technologien e.V. (Engl.Leibniz Institute of Photonic Technology) | USE OF ATOMIC THIN LAYERS OF TRANSITION METAL OXIDES AND/OR HYDROXIDES IN THE FORM OF ZN(OH)2 - ORIGAMI STRUCTURES |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1396117A (en) * | 2002-06-13 | 2003-02-12 | 山东小鸭集团有限责任公司 | Process for preparing nano zinc oxide |
| CN101823759A (en) * | 2010-04-01 | 2010-09-08 | 江苏工业学院 | Continuous large-area zinc oxide nano-sheet and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5440297A (en) * | 1977-09-06 | 1979-03-29 | Matsushita Electric Ind Co Ltd | Production of zinc hydroxide plate crystals |
| CN100494069C (en) * | 2006-12-21 | 2009-06-03 | 中国海洋石油总公司 | Preparing process of nano zinc oxide |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1396117A (en) * | 2002-06-13 | 2003-02-12 | 山东小鸭集团有限责任公司 | Process for preparing nano zinc oxide |
| CN101823759A (en) * | 2010-04-01 | 2010-09-08 | 江苏工业学院 | Continuous large-area zinc oxide nano-sheet and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| Studies on the adsorption of RuN3 dye on sheet-like nanostructured porous ZnO films;Rong Zhang et al.;《Solar Energy Materials & Solar Cells》;20071126;第92卷;425–431 * |
| 磷酸盐对水热和溶剂热合成的纳米氧化锌粉的影响;范学运等;《陶瓷学报》;20100930;第31卷(第3期);417-421 * |
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Inventor after: Sun Fengqiang Inventor after: Gu Kaiyuan Inventor after: Di Wei Inventor before: Sun Fengqiang Inventor before: Wu Chunsong Inventor before: Gu Kaiyuan Inventor before: Di Wei |
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