CN104741069B - A kind of preparation method of aluminum-doped zinc oxide nanometer powder - Google Patents
A kind of preparation method of aluminum-doped zinc oxide nanometer powder Download PDFInfo
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Abstract
The present invention relates to a kind of methods for producing aluminum-doped zinc oxide nanometer powder, belong to technical field of nanometer material preparation.Technical process are as follows: (1) by zinc nitrate, aluminum nitrate, amine organic matter and adjuvant wiring solution-forming according to a certain percentage；(2) solution is heated, is reacted after solution evaporation, concentration, obtain predecessor powder；(3) by predecessor powder in 400-800 DEG C of temperature range, it reacts 1-5 hours under air, it is simple to obtain aluminum-doped zinc oxide nanometer powder (4) present invention process, it is at low cost, it is easy to industrialization, the aluminum-doped zinc oxide nanometer powder crystal grain of preparation is tiny, good dispersion, granularity is controllable, has meso-hole structure, can be used for adsorbing the fields such as organic pollutant.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to a kind of aluminum-doped zinc oxide nanometer powder of producing
Method.
Background technique
Zinc oxide is a kind of n-type semiconductor of broad-band gap, forbidden bandwidth Eg=3.37eV at room temperature, has hexagonal
Wurtzite crystal structure is easy to produce defect and carries out impurity doping.Wherein aluminium-doped zinc oxide due to its distinctive structure and
Performance, make its light, electricity, magnetic, in terms of show excellent characteristic, be widely used in photoelectric material, photocatalysis
Agent, material obsorbing radar waves, ultraviolet light screener, sensor material and anti-biotic material preparation in, before having wide application
Scape.And be alternatively arranged as plastics, coating, fiber and other material a kind of functional filler, can assign that its is antistatic, electromagnetic shielding etc.
Performance.Furthermore the aluminum-doped zinc oxide nanometer powder with meso-hole structure is alternatively arranged as the adsorbent material of organic pollutant, application
In fields such as chemical industry, environmental protection, medical and health and bioengineering.
The method for wherein preparing doping zinc-oxide mainly has hydro-thermal method, coprecipitation, chemical vapour deposition technique etc..Chen Zhiwu
Deng the method for preparing aluminum-doped zinc oxide nanometer powder disclosed in the patent in publication number CN103496732A are as follows: with acetic acid
Zinc and aluminum nitrate are raw material, zinc acetate and aluminum nitrate are put into beaker, the mixing for adding ethylene glycol monomethyl ether and ethanol amine is molten
Liquid is made into uniform colloidal sol by magnetic agitation.The colloidal sol of generation is put into baking oven, obtains xerogel after dry, and through grinding
Mill obtains dry gel powder, i.e. hydro-thermal reaction predecessor；The hydro-thermal reaction predecessor of preparation is put into water heating kettle, and is added anhydrous
Ethyl alcohol is as solvent and NaOH as mineralizer.Reaction kettle is sealed, reaction kettle is placed in 120 DEG C~180 DEG C baking ovens, instead
Should after take out product, through sediment is obtained by filtration；Sediment is washed, obtains aluminium-doped zinc oxide powder after dry.Liu Shimin
Deng the method for preparing aluminum-doped zinc oxide nanometer powder disclosed in the patent in publication number CN103395826A are as follows: close first
At zinc nitrate out-urea leucosol microemulsion.It is filtered after standing, aluminum nitrate is added in filtrate and forms nitric acid zinc-aluminium mixed liquor.
Sodium carbonate liquor is configured, in the double instillation polyvinyl alcohol water solutions of zinc nitrate aluminum solutions, synthesizes white precipitate presoma.It stood
Filter, filter cake elutes through deionized water, dries, being ground up, sieved, calcine after obtain aluminum-doped zinc oxide nanometer powder.Qiu Fagui etc. exists
The method of aluminum-doped zinc oxide nanometer powder is prepared disclosed in the patent of publication number CN102616829A are as follows: by zinc nitrate, nitre
Sour aluminium and citric acid or urea or carbohydrazide are put into beaker, wherein the molar ratio of nitrate and citric acid or urea or carbohydrazide
It is 0.5~1.2, deionized water is added in 0.5~5.0at% of aluminium content, and stirring dissolves it sufficiently, is subsequently placed in digital display constant temperature
Continuous heating stirs on magnetic stirring apparatus, and controls the temperature of solution between 60 DEG C~70 DEG C, until solution forms colloidal sol；Control
The temperature of colloidal sol processed is at 80 DEG C until the lurid gel of formation, stops heating stirring；Beaker equipped with gel is put into preheating
Into 180 DEG C of chamber type electric resistance furnaces and this temperature is maintained to stop heating after 3~5 hours, to its cooled to room temperature, taken out
Obtained precursor powder is placed in chamber type electric resistance furnace to precursor powder, 800 DEG C is warming up to the rate of 5 DEG C/min, protects
Temperature 2~4 hours, then cooled to room temperature, obtains aluminium-doped zinc oxide nano material.
The above method prepares aluminum-doped zinc oxide nanometer powder complex process, higher cost, and granularity, dispersibility be not easily-controllable
System.Therefore, it is necessary to explore a kind of at low cost, simple process, granularity is controllable, the high dispersive aluminium with meso-hole structure adulterates
The preparation method of zinc oxide nano-powder.
Summary of the invention
The present invention provides a kind of method that simple, efficient, low cost prepares aluminum-doped zinc oxide nanometer powder.
The process step of the invention is as follows:
1, by zinc nitrate, aluminum nitrate, amine organic matter and adjuvant wiring solution-forming according to a certain percentage, wherein aluminum nitrate with
The molar ratio of zinc nitrate is 0.005-0.15, and the molar ratio of amine organic matter and zinc nitrate is 3-6, and adjuvant and zinc nitrate rub
You are than being 0.1-1；
2, the solution for forming step 1 heats, and reacts after solution evaporation, concentration, obtains predecessor powder；
3, predecessor powder is reacted 1-5 hours under air in 400-800 DEG C of temperature range, obtains aluminium doping oxygen
Change zinc nanometer powder.
4, amine organic matter described in step 1 is at least one of urea, glycine；Adjuvant is glucose, lemon
One of acid, sucrose.
The invention has the advantages that
1, precursor powder is prepared using the pyrolytic reaction between raw material each in liquid phase, it is simple process, quick, it can be
It is completed in more than ten minutes
2, the bulk gas released in each raw material reaction process can effectively prevent powder product to reunite；
3, the addition of adjuvant, can reduce reaction temperature, so that reaction becomes mild controllable.And in subsequent heat treatment mistake
The effect of dispersing agent is served as in journey, is prevented powder from reuniting and is grown up；
4, each raw material is mixed using liquid phase, it can be achieved that uniform in molecule rank of aluminum nitrate and zinc nitrate mixes, favorably
Aluminium element is uniformly distributed in product；
5, the controllable aluminium-doped zinc oxide of granularity can be obtained by adjusting proportion and the subsequent heat temperature of raw material
Nano-powder；
6, prepared aluminum-doped zinc oxide nanometer powder purity is high, good dispersion and has meso-hole structure, adsorbs organic dirt
It is high-efficient to contaminate object；
7, equipment is simple, and process flow is short, high-efficient, at low cost, is suitble to scale industrial production.
Detailed description of the invention
Fig. 1 is the XRD diagram of aluminum-doped zinc oxide nanometer powder of the present invention (aluminium doping is 4mol%).
Fig. 2 is that the EDS of aluminum-doped zinc oxide nanometer powder of the present invention (aluminium doping is 4mol%) schemes.
Fig. 3 is that the TEM of aluminum-doped zinc oxide nanometer powder of the present invention (aluminium doping is 4mol%) schemes
Fig. 4 is the nitrogen adsorption desorption curve graph of aluminum-doped zinc oxide nanometer powder of the present invention (aluminium doping is 4mol%).
Fig. 5 is absorption property figure (the 1g/L suction of aluminum-doped zinc oxide nanometer powder of the present invention (aluminium doping is 4mol%)
Attached dose, 50ppm methyl orange pollutant)
Specific embodiment
Embodiment 1
0.1 mole of zinc nitrate, 0.002 mole of aluminum nitrate, 0.4 mole of urea are weighed, 0.03 mole of glucose is dissolved in distillation
In water, it is configured to solution, solution is placed on controllable temperature electric furnace and is heated.Solution decomposes after experience volatilization, concentration, obtains
Predecessor powder.Precursor powder is reacted 1 hour in furnace under the conditions of 700 DEG C, air atmosphere, is obtained with meso-hole structure
Aluminium-doped zinc oxide nanometer powder.Gained powder particle size is 30~60nm, and concentration is the adsorbent of 1g/L by 20ppm's
Methyl orange contaminant degradation needs 15min.
Embodiment 2
0.1 mole of zinc nitrate, 0.004 mole of aluminum nitrate, 0.42 mole of urea are weighed, 0.025 mole of glucose is dissolved in steaming
In distilled water, it is configured to solution, solution is placed on controllable temperature electric furnace and is heated.Solution decomposes after experience volatilization, concentration, obtains
To predecessor powder.Precursor powder is reacted 1 hour in furnace under the conditions of 700 DEG C, air atmosphere, obtains that there is mesoporous knot
The aluminium-doped zinc oxide nanometer powder of structure.Gained powder particle size is 20~50nm, and concentration is the adsorbent of 1g/L by 20ppm
Methyl orange contaminant degradation need 5min.
Embodiment 3
0.1 mole of zinc nitrate, 0.008 mole of aluminum nitrate, 0.43 mole of urea are weighed, 0.03 mole of glucose is dissolved in distillation
In water, it is configured to solution, solution is placed on controllable temperature electric furnace and is heated.Solution decomposes after experience volatilization, concentration, obtains
Predecessor powder.Precursor powder is reacted 1 hour in furnace under the conditions of 500 DEG C, air atmosphere, is obtained with meso-hole structure
Aluminium-doped zinc oxide nanometer powder.Gained powder particle size is 15~35nm, and concentration is the adsorbent of 1g/L by 20ppm's
Methyl orange contaminant degradation needs 3min.
Embodiment 4
0.1 mole of zinc nitrate, 0.004 mole of aluminum nitrate, 0.45 mole of urea are weighed, 0.03 mole of glucose is dissolved in distillation
In water, it is configured to solution, solution is placed on controllable temperature electric furnace and is heated.Solution decomposes after experience volatilization, concentration, obtains
Predecessor powder.Precursor powder is reacted 1 hour in furnace under the conditions of 500 DEG C, air atmosphere, is obtained with meso-hole structure
Aluminium-doped zinc oxide nanometer powder.Gained powder particle size is 10~35nm, and concentration is the adsorbent of 1g/L by 50ppm's
Methyl orange contaminant degradation needs 7min.
Claims (1)
1. a kind of preparation method of aluminum-doped zinc oxide nanometer powder, which is characterized in that
(1) by zinc nitrate, aluminum nitrate, urea and glucose wiring solution-forming according to a certain percentage, wherein aluminum nitrate and zinc nitrate
Molar ratio is 0.005-0.15, and the molar ratio of urea and zinc nitrate is 3-6, and the molar ratio of glucose and zinc nitrate is 0.1-1；
(2) solution is heated, is reacted after solution evaporation, concentration, completed in more than ten minutes, obtain predecessor powder；
(3) predecessor powder is reacted 1-5 hours under air in 400-800 DEG C of temperature range, obtains aluminium-doped zinc oxide
Nanometer powder；
Controllable granularity, favorable dispersibility can be produced by adjusting raw material, proportion and with meso-hole structure, are adsorbed with
The high-efficient aluminium-doped zinc oxide nanometer powder of machine pollutant.
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| CN105948809A (en) * | 2016-05-05 | 2016-09-21 | 陕西科技大学 | Preparation method of porous ZnO block material |
| CN108455873A (en) * | 2017-02-17 | 2018-08-28 | 新加坡科技研究局 | Aluminium-doped zinc oxide film and the method for forming it |
| US11964739B2 (en) | 2020-08-07 | 2024-04-23 | Roger K. Young | Coatings that reduce or prevent barnacle attachment to a marine structure |
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| CN101582333A (en) * | 2009-06-22 | 2009-11-18 | 杭州电子科技大学 | Preparation method for electrodes of dye-sensitized solar battery |
| CN101885508A (en) * | 2009-05-14 | 2010-11-17 | 中国科学院宁波材料技术与工程研究所 | Method for preparing zinc oxide-doped nano powder controllably on large scale |
| CN102616829A (en) * | 2012-04-17 | 2012-08-01 | 吉林大学 | Production method for aluminum-doped zinc oxide nanometer material |
| CN103570056A (en) * | 2013-11-22 | 2014-02-12 | 江苏省东泰精细化工有限责任公司 | Method for preparing conductive powder by recoating aluminum-doped nano zinc oxide with aluminum |
| CN105329944A (en) * | 2014-08-13 | 2016-02-17 | 南京理工大学 | Method for preparing chrome oxide nano-material |
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| CN101885508A (en) * | 2009-05-14 | 2010-11-17 | 中国科学院宁波材料技术与工程研究所 | Method for preparing zinc oxide-doped nano powder controllably on large scale |
| CN101582333A (en) * | 2009-06-22 | 2009-11-18 | 杭州电子科技大学 | Preparation method for electrodes of dye-sensitized solar battery |
| CN102616829A (en) * | 2012-04-17 | 2012-08-01 | 吉林大学 | Production method for aluminum-doped zinc oxide nanometer material |
| CN103570056A (en) * | 2013-11-22 | 2014-02-12 | 江苏省东泰精细化工有限责任公司 | Method for preparing conductive powder by recoating aluminum-doped nano zinc oxide with aluminum |
| CN105329944A (en) * | 2014-08-13 | 2016-02-17 | 南京理工大学 | Method for preparing chrome oxide nano-material |
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