CN102757085A - Process for preparing nanometer zinc oxide with sol-gel process - Google Patents
Process for preparing nanometer zinc oxide with sol-gel process Download PDFInfo
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- CN102757085A CN102757085A CN2011101100713A CN201110110071A CN102757085A CN 102757085 A CN102757085 A CN 102757085A CN 2011101100713 A CN2011101100713 A CN 2011101100713A CN 201110110071 A CN201110110071 A CN 201110110071A CN 102757085 A CN102757085 A CN 102757085A
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Abstract
The invention aims to overcome the defects of high raw material cost, large contraction of gel volume during drying and calcining, easiness in causing aggregation among nanometer zinc oxide particles and the like existing in the conventional method, and provides a novel production method for preparing nanometer zinc oxide with a sol-gel process. A nanometer zinc oxide power crystal is 40-280 nanometers in size, and has the advantages of high purity, good crystal form and high dispersing property; and more importantly, a preparation method adopted in the invention has the advantages of saving in energy and higher safety. The process can be applied to the industries of rubber, paint, coatings, printing and dyeing, glass, medicine, cosmetics, electrons and the like.
Description
[technical field]
The present invention relates to a kind of technical field of semiconductors, specifically is a kind of nanometer Zinc oxide powder sol-gel method for preparing.
[background technology]
Nano zine oxide is a kind of novel inorganic functional materials of developing in recent years, and its size of particles is at 1～100nm.Because the granular of crystal grain; Its surface electronic structure and crystalline structure change; Characteristics such as the surface effects that macro object did not have, volume effect, quantum size effect and macroscopical tunnel effect and high-clarity, polymolecularity have been produced; At aspects such as magnetic, light, electric sensitivities, have common zinc oxide incomparable property, therefore have purposes widely.Nano zine oxide is mainly used in industry such as rubber, paint, coating, printing and dyeing, glass, medicine, makeup and electronics, as antimicrobial additive, sun-screening agent, photocatalyst, gas sensor, image recording material, absorbing material, electro-conductive material, piezoelectric, rubber accelerator etc.Along with reducing of superfine powder particle diameter; Its specific surface area increases thereupon and along with the powder surface atomicity is doubled and redoubled, particle surface can sharply increase, thereby makes that adsorption is strengthened between particle; Form aggregate, have a strong impact on the performance of superfine powder and the finished product.Experimental study finds that the pattern of zinc oxide and granularity have very big inheritance to the pattern and the granularity of zinc oxide precursor.Therefore, the preparation section of presoma is the key that influences the zinc oxide performance.Sol-gel method makes colloidal sol through hydrolysis and polycondensation, and further polycondensation obtains gel again.Gel obtains nano zine oxide through dry, calcining.The purity of this raw materials technology is higher, and whole process is not introduced foreign ion, can be through strict CONTROL PROCESS condition, make that purity height, particle diameter are little, the nano-powder of narrow particle size distribution, and constant product quality.
[summary of the invention]
It is high to the objective of the invention is to overcome existing method raw materials cost, and gel volume shrinks greatly during dry, calcining, is prone to cause the defectives such as reunion between nano granular of zinc oxide, and a kind of new nano zine oxide sol-gel method production technique is provided.Working method of the present invention is simple, and cost is low, and purity is done, and can realize industrialization production; Nanometer Zinc oxide powder of the present invention has purity height, good, the good dispersivity characteristic of crystal formation.
The present invention realizes through following technical scheme:
Nano zine oxide sol-gel method method production technique involved in the present invention includes following steps:
Step 1 takes by weighing an amount of Zinc diacetate dihydrate and is dissolved in wiring solution-forming in the certain volume deionized water;
Step 2 takes by weighing an amount of complexing agent and is dissolved in the certain volume absolute ethyl alcohol, and enveloping agent solution is heated to certain temperature;
Step 3, the solution of mixing step one and step 2 difference gained;
Step 4 adds compound surfactant, magnetic agitation in the solution of step 3 gained;
Step 5, the slow oxalic acid solution that drips certain volume makes it become the leucosol shape in step 4 gained solution;
Step 6 is incubated certain hour with the colloidal sol of step 5 gained, at a certain temperature up to making colloidal sol become gel;
Step 7 is inserted vacuum drying oven with the gel of step 6 gained, and dry at a certain temperature certain hour makes gel become xerogel fully;
Step 8 moves into the xerogel of step 7 gained in the retort furnace, and calcine at a certain temperature certain hour both nanometer Zinc oxide powder.
In the step 2, said complexing agent includes but not limited to oxalic acid, Hydrocerol A, Triammonium citrate, Triple Pressed Stearic Acid etc.
In the step 2, Heating temperature is at 65 ℃-80 ℃.
In the step 4, said compound surfactant is 1: 1 mixed in molar ratio gained of sodium lauryl sulphate and polyethylene glycol 6000, X 2073 and polyethylene glycol 6000.
In the step 6, holding temperature is at 60 ℃-80 ℃, and soaking time is at 4h-6h.
In the step 7, drying temperature is at 55 ℃-75 ℃, and soaking time is at 12h-20h.
In the step 8, calcining temperature is at 400 ℃-700 ℃, and soaking time is at 2h-5h.
The present invention has following beneficial effect: its nanometer Zinc oxide powder crystalline size is 40 nanometers-280 nanometers, has that purity height, crystal formation are good, the characteristic of good dispersivity; What is more important, the preparation method that the present invention adopted has saved the energy, and safer.
[embodiment]
Below in conjunction with embodiment the present invention is described further.Production technology of the present invention is to implement easily to this professional people.Present embodiment provided detailed embodiment and process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.
Embodiment
Claim that Zinc diacetate dihydrate 3.1g is dissolved in wiring solution-forming in the 67mL deionized water.
Claim that an amount of oxalic acid is dissolved in the 136mL absolute ethyl alcohol, is heated to enveloping agent solution about 70 ℃.
The adding mol ratio is 1: 1 X 2073 and a polyethylene glycol 6000 compound surfactant, and magnetic agitation slowly drips oxalic acid solution again, becomes leucosol.
Leucosol is incubated 6h about 65 ℃, colloidal sol becomes gel.
Gel is put in the vacuum drying oven to descend about dry 18h at 65 ℃, and gel becomes xerogel.
Xerogel is calcined 4h down at 500 ℃ get nanometer Zinc oxide powder.
The nanometer Zinc oxide powder crystalline size that present embodiment obtains is between 30nm-40nm.
Utilize above-mentioned sol-gel process can prepare nanometer Zinc oxide powder, and reach its distinctive beneficial effect.
Claims (8)
1. the present invention is a kind of technology of Prepared by Sol Gel Method nano zine oxide.The present invention has following beneficial effect: its nanometer Zinc oxide powder crystalline size is 40 nanometers-280 nanometers, has that purity height, crystal formation are good, the characteristic of good dispersivity
2. the technology of a kind of Prepared by Sol Gel Method nano zine oxide according to claim 1 comprises the steps:
Step 1 takes by weighing an amount of Zinc diacetate dihydrate and is dissolved in wiring solution-forming in the certain volume deionized water;
Step 2 takes by weighing an amount of complexing agent and is dissolved in the certain volume absolute ethyl alcohol, and enveloping agent solution is heated to certain temperature;
Step 3, the solution of mixing step one and step 2 difference gained;
Step 4 adds compound surfactant, magnetic agitation in the solution of step 3 gained;
Step 5, the slow oxalic acid solution that drips certain volume makes it become the leucosol shape in step 4 gained solution;
Step 6 is incubated certain hour with the colloidal sol of step 5 gained, at a certain temperature up to making colloidal sol become gel;
Step 7 is inserted vacuum drying oven with the gel of step 6 gained, and dry at a certain temperature certain hour makes gel become xerogel fully;
Step 8 moves into the xerogel of step 7 gained in the retort furnace, and calcine at a certain temperature certain hour both nanometer Zinc oxide powder.
3. the technology of a kind of Prepared by Sol Gel Method nano zine oxide according to claim 2 is characterized in that in the step 2 that said complexing agent includes but not limited to oxalic acid, Hydrocerol A, Triammonium citrate, Triple Pressed Stearic Acid etc.
4. the technology of a kind of Prepared by Sol Gel Method nano zine oxide according to claim 2 is characterized in that in the step 2, and Heating temperature is at 65 ℃-80 ℃.
5. the technology of a kind of Prepared by Sol Gel Method nano zine oxide according to claim 2 is characterized in that in the step 4, and said compound surfactant is 1: 1 mixed in molar ratio gained of sodium lauryl sulphate and polyethylene glycol 6000.
6. the technology of a kind of Prepared by Sol Gel Method nano zine oxide according to claim 2 is characterized in that in the step 6, and holding temperature is at 60 ℃-80 ℃, and soaking time is at 4h-6h.
7. the technology of a kind of Prepared by Sol Gel Method nano zine oxide according to claim 2 is characterized in that in the step 7, and drying temperature is at 55 ℃-75 ℃, and soaking time is at 12h-20h.
8. the technology of a kind of Prepared by Sol Gel Method nano zine oxide according to claim 2 is characterized in that in the step 8, and calcining temperature is at 400 ℃-700 ℃, and soaking time is at 2h-5h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011101100713A CN102757085A (en) | 2011-04-28 | 2011-04-28 | Process for preparing nanometer zinc oxide with sol-gel process |
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| CN2011101100713A CN102757085A (en) | 2011-04-28 | 2011-04-28 | Process for preparing nanometer zinc oxide with sol-gel process |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104264281A (en) * | 2014-09-17 | 2015-01-07 | 句容亿格纳米材料厂 | Preparation method of nanofibers |
| CN104307501A (en) * | 2014-10-31 | 2015-01-28 | 西南民族大学 | Method for preparing nano-zinc oxide used as photocatalyst |
| CN104722291A (en) * | 2015-04-01 | 2015-06-24 | 安徽工程大学 | Preparation method of nano zinc oxide glass fiber composite material |
| CN106006708A (en) * | 2016-05-23 | 2016-10-12 | 渤海大学 | Preparation method of lengthened octahedral hierarchical structure material of ZnO |
| CN106242020A (en) * | 2016-09-21 | 2016-12-21 | 沈阳工业大学 | A kind of zno-based composite catalyst and the method for hydrogen peroxide synergism photocatalysis degradation organic contaminant |
| CN108440855A (en) * | 2018-03-29 | 2018-08-24 | 青岛元汇丰企业管理咨询服务有限公司 | A kind of UV resistance culture dish and preparation method thereof |
| CN109721094A (en) * | 2019-02-27 | 2019-05-07 | 西南科技大学 | A kind of preparation method preparing zinc-oxide nano colloidal solution |
| CN109830586A (en) * | 2019-02-19 | 2019-05-31 | 芜湖德豪润达光电科技有限公司 | The preparation method and light emitting diode of transparency conducting layer |
| CN109935735A (en) * | 2017-12-15 | 2019-06-25 | Tcl集团股份有限公司 | A kind of ZnO film and preparation method thereof and QLED device |
| CN110006958A (en) * | 2019-04-10 | 2019-07-12 | 河北工业大学 | Co3O4The preparation method of ZnO nano material acetone thick film gas-sensitive sensor |
| CN111924872A (en) * | 2020-08-10 | 2020-11-13 | 东莞世皓新材料生物科技有限公司 | Method for preparing modified nano zinc oxide by sol-gel process |
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2011
- 2011-04-28 CN CN2011101100713A patent/CN102757085A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104264281B (en) * | 2014-09-17 | 2016-06-29 | 句容亿格纳米材料厂 | A kind of preparation method of nanofiber |
| CN104264281A (en) * | 2014-09-17 | 2015-01-07 | 句容亿格纳米材料厂 | Preparation method of nanofibers |
| CN104307501A (en) * | 2014-10-31 | 2015-01-28 | 西南民族大学 | Method for preparing nano-zinc oxide used as photocatalyst |
| CN104722291B (en) * | 2015-04-01 | 2017-05-17 | 安徽工程大学 | Preparation method of nano zinc oxide glass fiber composite material |
| CN104722291A (en) * | 2015-04-01 | 2015-06-24 | 安徽工程大学 | Preparation method of nano zinc oxide glass fiber composite material |
| CN106006708A (en) * | 2016-05-23 | 2016-10-12 | 渤海大学 | Preparation method of lengthened octahedral hierarchical structure material of ZnO |
| CN106006708B (en) * | 2016-05-23 | 2017-10-31 | 渤海大学 | A kind of zinc oxide elongates the preparation method of octahedra hierarchical organization material |
| CN106242020A (en) * | 2016-09-21 | 2016-12-21 | 沈阳工业大学 | A kind of zno-based composite catalyst and the method for hydrogen peroxide synergism photocatalysis degradation organic contaminant |
| CN106242020B (en) * | 2016-09-21 | 2019-06-25 | 沈阳工业大学 | A kind of method of zno-based composite catalyst and hydrogen peroxide synergistic effect photocatalysis degradation organic contaminant |
| CN109935735A (en) * | 2017-12-15 | 2019-06-25 | Tcl集团股份有限公司 | A kind of ZnO film and preparation method thereof and QLED device |
| CN108440855A (en) * | 2018-03-29 | 2018-08-24 | 青岛元汇丰企业管理咨询服务有限公司 | A kind of UV resistance culture dish and preparation method thereof |
| CN109830586A (en) * | 2019-02-19 | 2019-05-31 | 芜湖德豪润达光电科技有限公司 | The preparation method and light emitting diode of transparency conducting layer |
| CN109721094A (en) * | 2019-02-27 | 2019-05-07 | 西南科技大学 | A kind of preparation method preparing zinc-oxide nano colloidal solution |
| CN110006958A (en) * | 2019-04-10 | 2019-07-12 | 河北工业大学 | Co3O4The preparation method of ZnO nano material acetone thick film gas-sensitive sensor |
| CN111924872A (en) * | 2020-08-10 | 2020-11-13 | 东莞世皓新材料生物科技有限公司 | Method for preparing modified nano zinc oxide by sol-gel process |
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Application publication date: 20121031 |