CN102219252A - Process for preparing nanometer zinc-oxide by ultrasonic emulsification method - Google Patents
Process for preparing nanometer zinc-oxide by ultrasonic emulsification method Download PDFInfo
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- CN102219252A CN102219252A CN2010101502401A CN201010150240A CN102219252A CN 102219252 A CN102219252 A CN 102219252A CN 2010101502401 A CN2010101502401 A CN 2010101502401A CN 201010150240 A CN201010150240 A CN 201010150240A CN 102219252 A CN102219252 A CN 102219252A
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- ultrasonic method
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- zinc
- oxidized zinc
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Abstract
The invention discloses a process for preparing nanometer zinc-oxide by an ultrasonic emulsification method. The zinc-oxide powder obtained by the process has small granularity and rarely has crystal imperfection, meanwhile, the process adopted in the invention is simple to operate, and the nanometer zinc-oxide particles of different sizes can be obtained by changing the concentration ratio of reactants or changing the calcining temperature of precursors. The crystal size of the obtained nanometer zinc-oxide powder is about 20nm to 30nm. The process disclosed by the invention can be widely used for a solar energy device, a piezoelectric device, and the like.
Description
[technical field]
The present invention relates to a kind of technical field of semiconductor, specifically is that a kind of emulsification ultrasonic method prepares nano oxidized zinc technology.
[background technology]
Zinc oxide is a kind of important broad stopband direct band gap (E=3.37eV) semiconductor material, has wurtzite structure, at room temperature has bigger exciton bind energy (60meV), far above GaN exciton bind energy (21～25meV), and obtained widely using with its unique photoelectric properties.Therefore, zinc oxide is as new generation broadband gap semiconductor compound-material, owing to the morphological structure that itself has good photoelectric property and enrich receives much concern.Simultaneously, nano zine oxide presents the not available property of conventional oxidation zinc: nontoxic and non-migrating, fluorescence, piezoelectricity, absorption and scatters ultraviolet ability etc. have vital role for improving photoelectric device, ultraviolet laser performance and photocatalyst efficient.At present, zinc oxide is obtained application at aspects such as photoelectric instrument, piezo-electric apparatus, transmitter, photocatalytic device and a large amount of acoustic wave apparatus, and nano zine oxide can be widely used in fields such as rubber, daily-use chemical industry, medicine, magneticsubstance as a kind of non-toxic material.Over past ten years, the research report of relevant nano zine oxide preparation both at home and abroad is more.Make a general survey of all documents, wherein relatively have the preparation method of application prospect to mainly contain the precipitator method, sol-gel method, hydrothermal method, electrochemical deposition method, solid reaction process and mini-emulsion process etc.
[summary of the invention]
Cavitation, pulverizing, dissemination that the present invention's comprehensive nonionic surface active agent good emulsifying dissemination and ultrasonic radiation are strong, on the basis of document in early stage, attempt under normal temperature, normal pressure, having prepared the nano ZnO powder of multiple granularity for the first time, a kind of nanometer Zinc oxide powder emulsification-ultrasonic method production technique is provided with emulsification-ultrasonic method.The present invention has simple, easy to operate, the advantages such as dosage of surfactant is few, good stability of experimental installation, overcome particle size that the traditional precipitator method exist and be difficult to control, easily reunite and shortcoming such as size-grade distribution is inhomogeneous, had industry and promote and actual application value.
Nanometer Zinc oxide powder of the present invention has the controlled characteristic of epigranular.
The present invention is achieved by the following technical solutions:
Emulsification ultrasonic method involved in the present invention prepares nano oxidized zinc technology, comprises the steps:
Step 1 takes by weighing a certain amount of Zinc Sulphate Heptahydrate wiring solution-forming in beaker;
Step 2 adds a certain amount of Triton X-100 and vigorous stirring in the solution that step 1 obtains;
Step 3 takes by weighing a certain amount of NH
4HCO
3And be dissolved in wiring solution-forming in the beaker;
Step 4, the solution that step 3 and step 4 are obtained mixes under intense stirring condition, and continues to stir the regular hour;
The solution that step 5, step 4 obtain is static to spend the night, and removes supernatant liquid, and precipitation is placed beaker;
The precipitation supersound process certain hour that step 6, step 5 obtain;
The precipitation that step 7, step 6 obtain is washed till the sulfate radical-free ion with distilled water;
The precipitation that step 8, step 7 obtain is the freeze-day with constant temperature certain hour at a certain temperature, obtains the precursor zinc subcarbonate;
The calcining certain hour had both got the desired product nano zine oxide in the precursor that step 9, step 8 the obtain retort furnace at a certain temperature.
Wherein
In the step 2, the volume percent of the Triton X-100 of adding is 0.2%.
In the step 4, churning time is at 4h-6h.
In the step 6, the supersound process time is at 1h-2h.
In the step 7, sulfate ion 0.1mol/L BaCl
2Check.
In the step 8, drying temperature is 80 ℃-100 ℃, and be 2h-4h time of drying.
In the step 9, calcining temperature is 300 ℃-800 ℃, and calcination time is 2h-4h.
The present invention has following beneficial effect: it is little that its Zinc oxide powder has granularity, almost do not have the characteristic of lattice defect; Simultaneously, technological operation of the present invention is simple also can be by changing the calcining temperature of concentration of reactants proportioning or change precursor, to obtain the nano granular of zinc oxide of different size.
[embodiment]
The invention will be further described below in conjunction with embodiment.Production technology of the present invention is implemented easily to the people of material specialty.Present embodiment has provided detailed embodiment and process being to implement under the prerequisite with the technical solution of the present invention, but protection scope of the present invention includes but not limited to following embodiment.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or manufacturer's condition of advising.
Embodiment
Quantitatively take by weighing the 10g Zinc Sulphate Heptahydrate and be dissolved in the 200ml beaker, and the adding volume percent is 0.2%Triton X-100 under stirring condition.
Quantitatively take by weighing 25g bicarbonate of ammonia and be dissolved in the 200ml beaker, and under stirring condition with above-mentioned solution thorough mixing.Stir 5h, static spending the night.
Remove the upper strata stillness of night, obtain lower sediment, precipitation is placed beaker.
Ultrasonication precipitation 2h, then repeatedly with the distilled water wash precipitation, up to there not being sulfate ion residual.Suction filtration separates, and at 100 ℃ of dry 3h, obtains the precursor zinc subcarbonate.
The precursor zinc subcarbonate is calcined 2h under 600 ℃ of retort furnaces, obtain our product.
The nanometer Zinc oxide powder crystalline size that present embodiment obtains is between 20nm-30nm.
Utilize aforesaid method can prepare nanometer Zinc oxide powder, and reach its distinctive beneficial effect.
Claims (8)
1. the present invention is that a kind of emulsification ultrasonic method prepares nano oxidized zinc technology.Zinc oxide product of the present invention has good toughness, and the nanometer Zinc oxide powder crystalline size that obtains is between 20nm-30nm.
2. a kind of emulsification ultrasonic method according to claim 1 prepares nano oxidized zinc technology, comprises the steps:
Step 1 takes by weighing a certain amount of Zinc Sulphate Heptahydrate wiring solution-forming in beaker;
Step 2 adds a certain amount of Triton X-100 and vigorous stirring in the solution that step 1 obtains;
Step 3 takes by weighing a certain amount of NH
4HCO
3And be dissolved in wiring solution-forming in the beaker;
Step 4, the solution that step 3 and step 4 are obtained mixes under intense stirring condition, and continues to stir the regular hour;
The solution that step 5, step 4 obtain is static to spend the night, and removes supernatant liquid, and precipitation is placed beaker;
The precipitation supersound process certain hour that step 6, step 5 obtain;
The precipitation that step 7, step 6 obtain is washed till the sulfate radical-free ion with distilled water;
The precipitation that step 8, step 7 obtain is the freeze-day with constant temperature certain hour at a certain temperature, obtains the precursor zinc subcarbonate;
The calcining certain hour had both got the desired product nano zine oxide in the precursor that step 9, step 8 the obtain retort furnace at a certain temperature.
3. a kind of emulsification ultrasonic method according to claim 2 prepares nano oxidized zinc technology, it is characterized in that in the step 2, and the volume percent of the Triton X-100 of adding is 0.2%.
4. a kind of emulsification ultrasonic method according to claim 2 prepares nano oxidized zinc technology, it is characterized in that in the step 4, churning time is at 4h-6h.
5. a kind of emulsification ultrasonic method according to claim 2 prepares nano oxidized zinc technology, it is characterized in that in the step 6 that the supersound process time is at 1h-2h.
6. a kind of emulsification ultrasonic method according to claim 2 prepares nano oxidized zinc technology, it is characterized in that in the step 7 sulfate ion 0.1mol/L BaCl
2Check.
7. a kind of emulsification ultrasonic method according to claim 2 prepares nano oxidized zinc technology, it is characterized in that in the step 8, and drying temperature is 80 ℃-100 ℃, and be 2h-4h time of drying.
8. a kind of emulsification ultrasonic method according to claim 2 prepares nano oxidized zinc technology, it is characterized in that in the step 9, and calcining temperature is 300 ℃-800 ℃, and calcination time is 2h-4h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101502401A CN102219252A (en) | 2010-04-16 | 2010-04-16 | Process for preparing nanometer zinc-oxide by ultrasonic emulsification method |
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| CN2010101502401A CN102219252A (en) | 2010-04-16 | 2010-04-16 | Process for preparing nanometer zinc-oxide by ultrasonic emulsification method |
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| CN2010101502401A Pending CN102219252A (en) | 2010-04-16 | 2010-04-16 | Process for preparing nanometer zinc-oxide by ultrasonic emulsification method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105692686A (en) * | 2016-04-28 | 2016-06-22 | 北京化工大学常州先进材料研究院 | Preparation method of nanometer zinc oxide powder |
| RU2741913C1 (en) * | 2020-04-30 | 2021-01-29 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Вятский государственный университет" | Zinc carbonate production method |
-
2010
- 2010-04-16 CN CN2010101502401A patent/CN102219252A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105692686A (en) * | 2016-04-28 | 2016-06-22 | 北京化工大学常州先进材料研究院 | Preparation method of nanometer zinc oxide powder |
| CN105692686B (en) * | 2016-04-28 | 2017-11-17 | 北京化工大学常州先进材料研究院 | A kind of preparation method of nanometer Zinc oxide powder |
| RU2741913C1 (en) * | 2020-04-30 | 2021-01-29 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Вятский государственный университет" | Zinc carbonate production method |
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Application publication date: 20111019 |