CN101857428A - Preparation method of conductive zinc oxide powder - Google Patents
Preparation method of conductive zinc oxide powder Download PDFInfo
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- CN101857428A CN101857428A CN201010182261A CN201010182261A CN101857428A CN 101857428 A CN101857428 A CN 101857428A CN 201010182261 A CN201010182261 A CN 201010182261A CN 201010182261 A CN201010182261 A CN 201010182261A CN 101857428 A CN101857428 A CN 101857428A
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Abstract
The invention belongs to the technical field of inorganic chemistry, in particular to a preparation method of conductive zinc oxide powder materials. The invention adopts a sol-gal method combined with ultrasonic waves and microwaves for preparation. Corresponding zinc sources, aluminum sources and dispersing agents are put into a reaction vessel, water is used as a medium for efficiently obtaining gel state predecessors with uniform doping effect and stable property through the unique effects of the ultrasonic waves and the microwaves, and then, the gel state predecessors are calcined at a certain temperature to prepare the aluminum-oxide-doping conductive zinc oxide powder. The prepared powder has the advantages of good dispersivity, small grain diameter, uniform size direction, good conductive performance, high chemical stability and the like, and can be widely applied to various fields such as antistatic floor paint, anticorona paint and the like.
Description
Technical field
The invention belongs to domain of inorganic chemistry, be specifically related to a kind of preparation method of conductive zinc oxide powder.
Background technology
Zinc oxide is the extremely wide semiconductor material of a kind of range of application, and band gap is 3.37eV under its room temperature, and exciton bind energy is up to 60meV.Al-Doped ZnO (ZAO) is the substitutional solid solution that zinc oxide and aluminum oxide form, and has of light color, characteristics such as visible light transmissivity is high, good conductivity.Utilize its prepared conduction ZAO powder to have good electrical conductivity and dispersiveness, can be widely used in numerous areas such as antistatic terrace lacquer and anticorona coating.
At present, though the existing coprecipitation method (EP-A-404087) of preparation method of conduction ZAO powder, the ultrasound templates method (Luo Chongxiao, etc.Acta PhySico-Chimica Sinica, 2008,24 (6): 1007-1011) etc.; But in field of inorganic material preparing technology, be widely used, obtain product dispersing property sol-gel method preferably, but never be applied to conducting electricity the preparation of ZAO powder.The great advantage of sol-gel method is: raw materials used being dispersed to forms low viscous solution in the solvent, be easy to even, quantitative some trace elements that mix, realize the even doping on the molecular level, this will be very favourable to electroconductibility and the dispersiveness that improves conduction ZAO powder.But, utilizing sol-gel method, in the process of preparation conduction ZAO powder, main exist use comparatively that expensive organic solvents, reaction times are long, dissolved colloidal state many deficiencies such as need carry out to the transformation of gel state under the vacuum condition of harshness.This just causes in the process of industrialization conduction ZAO powder, and sol-gel method is difficult to be used, and can't reach the target that scientific research combines with practical application.Cause these insufficient major causes to be: 1. existing sol-gel method is general with an organic solvent as the medium of system, keeps the stable of sol system; 2. must make hydrolysis, condensation reaction be carried out slowly by leaving standstill for a long time, guarantee that in the precursor mix uniformly in the aluminium source; 3. change in the process of gel at colloidal sol, often be chosen under the vacuum condition, colloidal sol is carried out long oven drying at low temperature, avoid gel in forming process, the generation of the situations such as the inhomogeneous gel skeleton that causes caves in, contraction of being heated because of system.Therefore, present stage does not still have any about using sol-gel method to prepare the report appearance of conduction ZAO powder.
The present invention is directed to the deficiency of existing conduction ZAO powder preparing present situation, creatively proposed a kind of preparation method of new conduction ZAO powder, i.e. the sol-gel method that employing combines with ultrasonic wave, microwave.This method is conceived to improve the electroconductibility and the dispersiveness of conduction ZAO powder, under the prerequisite that keeps sol-gel method self advantage, improve reaction efficiency greatly, avoided the use of complicated vacuum dryer, made the industrialization of conduction ZAO powder become possibility; And, do not add any organic solvent in the reaction, when reducing production costs, meet the Green Chemistry requirement.The cavitation whirlpool that the present invention forms by ultrasonic wave dexterously quickens the mass transfer process between the interface, when keeping the sol system stable existence, improved the speed of raw material generation hydrolysis, condensation reaction; The present invention also utilizes the intramolecule rapid heating characteristic of microwave, change in the process of gel at colloidal sol, even, the flash baking of gel have been guaranteed, both can avoid caving in of gel skeleton, keep the complete of gel structure, shorten the time of gel formation again, improved the speed of entire reaction; The adding of dispersion agent has further improved the homogeneity of aluminium source doping in the precursor, makes system can better form sosoloid, has alleviated interparticle reunion to a certain extent, reaches the effect that improves product dispersiveness, control product size.The preparation effect that sol-gel method after this improvement obtains is that existing conductive zinc oxide powder preparation method is difficult to reach at aspects such as speed of reaction, product electric conductivity, dispersiveness and environment friendly.
Equipment is simple, combined coefficient is high, production cost is low because the preparation method that the present invention adopts has, the product good dispersity, electroconductibility is good and characteristics such as environmentally friendly, therefore, has very strong commercial viability.
Summary of the invention
The objective of the invention is to propose a kind of preparation method of conductive zinc oxide nano-powder, obtain the light color conducting nano powder that particle diameter is even, conductivity is good, solve the deficiency that the conductive powder body color of using in existing antistatic field is dark, be difficult for toning, reduce the production cost of conductive zinc oxide nano-powder simultaneously, realize the homogeneous and controllable of product size and distribution better.
The present invention proposes the preparation method of novel conduction ZAO powder, adopt improved sol-gel method to be prepared, its concrete steps are: will drop in the reactor as the starting material of zinc source, aluminium source and dispersion agent, be medium with water, is stirred well to raw material and all dissolves; Under the condition that ultrasonic wave exists, in system, slowly drip hydrazine hydrate, obtain the dissolved colloidal state precursor; To change in the microwave reactor behind the washing of dissolved colloidal state precursor, the suction filtration again, in microwave environment, obtain the gel state precursor; And then it is changed in the retort furnace calcine; Behind the naturally cooling, can obtain conductive zinc oxide powder;
Concrete preparation condition is:
The adding quality of dispersion agent: 0.5～10% of zinc source and aluminium source total mass;
The adding quality of hydrazine hydrate: the 1.25-2.0 of zinc source and aluminium source total mass doubly;
The calcining temperature of precursor: 500～800 ℃, calcination time 1～5h.
Affiliated tensio-active agent is nonionogenic tenside or anion surfactant.
The product of the present invention through obtaining after calcining, color is very light yellow powder, particle diameter reaches nanometer scale, and has good dispersiveness.
The present invention has following advantage:
1, propose to utilize improved sol-gel method to prepare conduction ZAO powder first.This method is compared with common sol-gel method, under the condition that keeps sol-gel method self advantage, utilized the unique effect of ultrasonic wave and microwave dexterously, the not only interpolation of no any organic reagent in preparation process, meet the Green Chemistry requirement, and reaction efficiency is greatly improved, also avoided the use of complicated vacuum dryer, save production cost greatly, possessed very strong commercial viability.
2, the adding of dispersion agent has further improved the homogeneity of aluminium source doping in the precursor, makes system can better form sosoloid, has alleviated interparticle reunion to a certain extent, reaches the effect that improves product dispersiveness, control product size.
3, the same co-precipitation of the product that utilizes the present invention to prepare, ultrasonic-additive methods such as template are compared, the conduction ZAO powder of preparation have the purity height, of light color, particle diameter is little and homogeneous, good, the no agglomeration of electroconductibility, be easy to advantages such as dispersion.
Embodiment
The present invention is further illustrated below by specific embodiment.
Embodiment 1:
Take by weighing Al (NO
3)
39H
2O 0.37g, Zn (NO
3)
26H
2O 14.6g, Triton x-1000.075g.Above-mentioned raw materials is all dropped in the reactor, add the 100mL deionized water, be stirred well to raw material and all dissolve as reaction medium; Under the condition that ultrasonic wave exists, in system, slowly drip hydrazine hydrate 29mL (density is 1.03g/mL, and reduced mass is 30g), fully react to system, obtain the dissolved colloidal state precursor after, stop hyperacoustic use, with colloidal sol washing, suction filtration; Again gained colloidal sol is placed microwave reactor, use the way of microwave drying, obtain the gel state precursor; Again the gel state precursor is put into retort furnace, calcining temperature is set to 700 ℃, behind the calcining 2h, naturally cool to room temperature, obtain light yellow conductive zinc oxide nano-powder, product has good electroconductibility and dispersiveness, and the particle diameter by the transmission electron microscope observation product is about 35nm.
Embodiment 2
Take by weighing Al
2(SO
4)
318H
2O 0.66g, ZnSO
47H
2O 14.1g, Triton x-1001.5g.Above-mentioned raw materials is all dropped in the reactor, add the 100mL deionized water, be stirred well to raw material and all dissolve as reaction medium; Under the condition that ultrasonic wave exists, in system, slowly drip hydrazine hydrate 14mL (density is 1.03g/mL, and reduced mass is 15g), fully react to system, obtain the dissolved colloidal state precursor after, stop hyperacoustic use, with colloidal sol washing, suction filtration; Again gained colloidal sol is placed microwave reactor, use the way of microwave drying, obtain the gel state precursor; Again the gel state precursor is put into retort furnace, calcining temperature is made as 500 ℃, behind the calcining 3h, naturally cool to room temperature, obtain light yellow conductive zinc oxide nano-powder, product has good electroconductibility and dispersiveness, and the particle diameter by the transmission electron microscope observation product is about 30nm.
Embodiment 3
Take by weighing AlCl
36H
2O 0.46g, ZnCl
213.4g, polyoxyethylene glycol 0.075g.Above-mentioned raw materials is all dropped in the reactor, add the 100mL deionized water, be stirred well to raw material and all dissolve as reaction medium; Under the condition that ultrasonic wave exists, in system, slowly drip hydrazine hydrate 19mL (density is 1.03g/mL, and reduced mass is 20g), fully react to system, obtain the dissolved colloidal state precursor after, stop hyperacoustic use, with colloidal sol washing, suction filtration; Again gained colloidal sol is placed microwave reactor, use the way of microwave drying, obtain the gel state precursor; Again the gel state precursor is put into retort furnace, calcining temperature is made as 800 ℃, behind the calcining 5h, naturally cool to room temperature, obtain light yellow conductive zinc oxide nano-powder, product has good electroconductibility and dispersiveness, and the particle diameter by the transmission electron microscope observation product is about 45nm.
Embodiment 4
Take by weighing Al (NO
3)
39H
2O 0.37g, Zn (NO
3)
26H
2O 14.6g, Sodium dodecylbenzene sulfonate 0.075g.Above-mentioned raw materials is all dropped in the reactor, add the 100mL deionized water, be stirred well to raw material and all dissolve as reaction medium; Under the condition that ultrasonic wave exists, in system, slowly drip hydrazine hydrate 19mL (density is 1.03g/mL, and reduced mass is 20g), fully react to system, obtain the dissolved colloidal state precursor after, stop hyperacoustic use, with colloidal sol washing, suction filtration; Again gained colloidal sol is placed microwave reactor, use the way of microwave drying, obtain the gel state precursor; Again the gel state precursor is put into retort furnace, calcining temperature is made as 600 ℃, behind the calcining 2h, naturally cool to room temperature, obtain light yellow conductive zinc oxide nano-powder, product has good electroconductibility and dispersiveness, and the particle diameter by the transmission electron microscope observation product is about 15nm.
Embodiment 5
Take by weighing Al (NO
3)
39H
2O 0.37g, Zn (NO
3)
26H
2O 14.6g, Sodium dodecylbenzene sulfonate 1.5g.Above-mentioned raw materials is all dropped in the reactor, add the 100mL deionized water, be stirred well to raw material and all dissolve as reaction medium; Under the condition that ultrasonic wave exists, in system, slowly drip hydrazine hydrate 29mL (density is 1.03g/mL, and reduced mass is 30g), fully react to system, obtain the dissolved colloidal state precursor after, stop hyperacoustic use, with colloidal sol washing, suction filtration; Again gained colloidal sol is placed microwave reactor, use the way of microwave drying, obtain the gel state precursor; Again the gel state precursor is put into retort furnace, calcining temperature is made as 600 ℃, behind the calcining 5h, naturally cool to room temperature, obtain light yellow conductive zinc oxide nano-powder, product has good electroconductibility and dispersiveness, and the particle diameter by the transmission electron microscope observation product is about 20nm.
Claims (6)
1. the preparation method of a conductive zinc oxide powder, it is characterized in that: employing is prepared with the sol-gel method that ultrasonic wave, microwave combine, concrete steps are: will drop into as the starting material of zinc source, aluminium source and dispersion agent in the reactor, with water is medium, is stirred well to raw material and all dissolves; Under the condition that ultrasonic wave exists, in system, slowly drip hydrazine hydrate, obtain the dissolved colloidal state precursor; To change in the microwave reactor behind the washing of dissolved colloidal state precursor, the suction filtration again, in microwave environment, obtain the gel state precursor; And then it is changed in the retort furnace calcine; Behind the naturally cooling, can obtain conductive zinc oxide powder;
Concrete preparation condition is:
The adding quality of dispersion agent: 0.5～10% of zinc source and aluminium source total mass;
The adding quality of hydrazine hydrate: the 1.0-2.0 of zinc source and aluminium source total mass doubly;
The calcining temperature of precursor: 500～800 ℃, calcination time 1～5h.
2. the preparation method of conductive zinc oxide powder according to claim 1, the ratio that it is characterized in that the amount of zinc atom and aluminium atom species is 100: 2.
3. the preparation method of conductive zinc oxide powder according to claim 1 is characterized in that the zinc source is zinc sulfate, zinc nitrate, zinc chloride.
4. the preparation method of conductive zinc oxide powder according to claim 1 is characterized in that the aluminium source is Tai-Ace S 150, aluminum nitrate, aluminum chloride,
Described tensio-active agent is nonionogenic tenside or anion surfactant.
5. the preparation method of conductive zinc oxide powder as claimed in claim 1, its spy is that described nonionogenic tenside is aliphatic alcohols, polyethylene glycols, polyvinyl alcohol, alcohol amide class, alkyl amine, alkylbenzene phenols.
6. the preparation method of conductive zinc oxide powder as claimed in claim 1, its spy is that described anion surfactant is carboxylate salt, phosphoric acid salt, vitriol, sulfonate.
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| CN201010182261A CN101857428A (en) | 2010-05-21 | 2010-05-21 | Preparation method of conductive zinc oxide powder |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220109A (en) * | 2011-04-25 | 2011-10-19 | 苏州晶讯科技股份有限公司 | Preparation method of sizing applied to electrostatic devices |
| CN102531038A (en) * | 2012-02-23 | 2012-07-04 | 华东理工大学 | Light color rodlike ZAO (Zinc Aluminium Oxide) conductive powder and preparation method thereof |
| CN104607216A (en) * | 2014-12-31 | 2015-05-13 | 华东理工大学 | One-step synthesis method of phosphorus-aluminum co-doped type conductive zinc oxide nanometer catalyst |
| CN105970323A (en) * | 2016-05-05 | 2016-09-28 | 苏州新民纺织有限公司 | Antistatic powder and preparation method thereof |
| CN108585503A (en) * | 2018-06-28 | 2018-09-28 | 中山市武汉理工大学先进工程技术研究院 | A kind of novel electrostatic prevention ceramic glaze and its preparation method and application |
| CN108821762A (en) * | 2018-06-28 | 2018-11-16 | 中山市武汉理工大学先进工程技术研究院 | A kind of antistatic Al-Doped ZnO conducting powder and its preparation method and application |
| CN109306234A (en) * | 2018-09-05 | 2019-02-05 | 纳琳威纳米科技南通有限公司 | A kind of antistatic coated film of long-acting type and preparation method thereof |
| CN112500152A (en) * | 2020-12-15 | 2021-03-16 | 无锡特科精细陶瓷有限公司 | Preparation method of anti-static ceramic |
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| CN1693279A (en) * | 2005-04-26 | 2005-11-09 | 黄德欢 | Process for preparing composite powder of nano copper-zine oxide |
| CN101531392A (en) * | 2009-03-27 | 2009-09-16 | 华东理工大学 | Preparation method of light color conducting nano powder material |
| CN101708829A (en) * | 2009-11-24 | 2010-05-19 | 华东理工大学 | Method for preparing yttria-stabilized zirconia powder |
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2010
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1693279A (en) * | 2005-04-26 | 2005-11-09 | 黄德欢 | Process for preparing composite powder of nano copper-zine oxide |
| CN101531392A (en) * | 2009-03-27 | 2009-09-16 | 华东理工大学 | Preparation method of light color conducting nano powder material |
| CN101708829A (en) * | 2009-11-24 | 2010-05-19 | 华东理工大学 | Method for preparing yttria-stabilized zirconia powder |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220109A (en) * | 2011-04-25 | 2011-10-19 | 苏州晶讯科技股份有限公司 | Preparation method of sizing applied to electrostatic devices |
| CN102220109B (en) * | 2011-04-25 | 2013-10-02 | 苏州晶讯科技股份有限公司 | Preparation method of sizing applied to electrostatic devices |
| CN102531038A (en) * | 2012-02-23 | 2012-07-04 | 华东理工大学 | Light color rodlike ZAO (Zinc Aluminium Oxide) conductive powder and preparation method thereof |
| CN102531038B (en) * | 2012-02-23 | 2013-12-25 | 华东理工大学 | Preparation method of light color rodlike ZAO (Zinc Aluminium Oxide) conductive powder |
| CN104607216B (en) * | 2014-12-31 | 2017-01-04 | 华东理工大学 | The one-step method for synthesizing of phosphorus aluminum codope type conductive zinc oxide nanocatalyst |
| CN104607216A (en) * | 2014-12-31 | 2015-05-13 | 华东理工大学 | One-step synthesis method of phosphorus-aluminum co-doped type conductive zinc oxide nanometer catalyst |
| CN105970323A (en) * | 2016-05-05 | 2016-09-28 | 苏州新民纺织有限公司 | Antistatic powder and preparation method thereof |
| CN105970323B (en) * | 2016-05-05 | 2018-04-13 | 吴江新民高纤有限公司 | A kind of antistatic powder and preparation method thereof |
| CN108585503A (en) * | 2018-06-28 | 2018-09-28 | 中山市武汉理工大学先进工程技术研究院 | A kind of novel electrostatic prevention ceramic glaze and its preparation method and application |
| CN108821762A (en) * | 2018-06-28 | 2018-11-16 | 中山市武汉理工大学先进工程技术研究院 | A kind of antistatic Al-Doped ZnO conducting powder and its preparation method and application |
| CN108585503B (en) * | 2018-06-28 | 2021-01-26 | 中山市武汉理工大学先进工程技术研究院 | Novel anti-static ceramic glaze and preparation method and application thereof |
| CN108821762B (en) * | 2018-06-28 | 2021-07-13 | 中山市武汉理工大学先进工程技术研究院 | Anti-static aluminum-doped zinc oxide conductive powder and preparation method and application thereof |
| CN109306234A (en) * | 2018-09-05 | 2019-02-05 | 纳琳威纳米科技南通有限公司 | A kind of antistatic coated film of long-acting type and preparation method thereof |
| CN112500152A (en) * | 2020-12-15 | 2021-03-16 | 无锡特科精细陶瓷有限公司 | Preparation method of anti-static ceramic |
| CN112500152B (en) * | 2020-12-15 | 2022-09-09 | 无锡特科精细陶瓷有限公司 | Preparation method of anti-static ceramic |
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Application publication date: 20101013 |