CN104741069A - Preparation method of aluminum-doped zinc oxide nano powder - Google Patents
Preparation method of aluminum-doped zinc oxide nano powder Download PDFInfo
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- CN104741069A CN104741069A CN201510128790.6A CN201510128790A CN104741069A CN 104741069 A CN104741069 A CN 104741069A CN 201510128790 A CN201510128790 A CN 201510128790A CN 104741069 A CN104741069 A CN 104741069A
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Abstract
The invention relates to a method for producing aluminum-doped zinc oxide nano powder, and belongs to the technical field of the preparation of a nano material. The preparation method comprises the following technological processes: (1) preparing a solution from zinc nitrate, aluminum nitrate, amine organic matters and adjuvant according to certain proportions; (2) heating the solution, and carrying out reaction after the solution is volatilized and concentrated so as to obtain precursor powder; and (3) reacting the precursor powder in air within a temperature range of 400-800 DEG C for 1-5h so as to obtain the aluminum-doped zinc oxide nano powder. The preparation method disclosed by the invention is simple in process, low in cost and easy in industrialization; and the prepared aluminum-doped zinc oxide nano powder is fine in crystalline grain, good in dispersity and controllable in grain size, and the nano powder has a mesoporous structure and is applicable to the fields of organic pollutant adsorption and the like.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, be specifically related to a kind of method of producing aluminum-doped zinc oxide nanometer powder.
Background technology
Zinc oxide is a kind of n-type semiconductor of broad-band gap, and its energy gap Eg=3.37eV at room temperature, has hexagonal wurtzite crystal structure, easily produces defect and carries out impurity doping.Wherein aluminium-doped zinc oxide is due to its distinctive stuctures and properties, make it in optical, electrical, magnetic, chemistry etc., show excellent characteristic, be widely used in the preparation of photoelectric material, photochemical catalyst, material obsorbing radar waves, ultraviolet light screener, sensor material and anti-biotic material, have broad application prospects.And also can be used as a kind of functional filler of plastics, coating, fiber and other material, the performances such as it is antistatic, electromagnetic shielding can be given.The aluminum-doped zinc oxide nanometer powder in addition with meso-hole structure also can be used as the sorbing material of organic pollution, is applied to the fields such as chemical industry, environmental protection, medical and health and bioengineering.
The method wherein preparing doping zinc-oxide mainly contains hydro-thermal method, coprecipitation, chemical vapour deposition technique etc.The method preparing aluminum-doped zinc oxide nanometer powder disclosed in the patent of publication number CN103496732A such as Chen Zhiwu is: with zinc acetate and aluminum nitrate for raw material, zinc acetate and aluminum nitrate are put into beaker, add the mixed solution of EGME and monoethanolamine again, be made into uniform colloidal sol by magnetic agitation.The colloidal sol of generation is put in baking oven, after drying, obtains xerogel, and obtain dry gel powder, i.e. hydro-thermal reaction predecessor through grinding; The hydro-thermal reaction predecessor of preparation is put into water heating kettle, and adds absolute ethyl alcohol as solvent, and NaOH is as mineralizer.Sealed reactor, is placed in reactor in 120 DEG C ~ 180 DEG C baking ovens, takes out product, be precipitated thing after filtration after reaction; Sediment, through washing, obtains aluminium-doped zinc oxide powder after drying.The method preparing aluminum-doped zinc oxide nanometer powder disclosed in the patent of publication number CN103395826A such as Liu Shimin is: first synthesize zinc nitrate-urea leucosol microemulsion.Filter after leaving standstill, add aluminum nitrate in filtrate and form nitric acid zinc-aluminium mixed liquor.Configuration sodium carbonate liquor, instills in polyvinyl alcohol water solution with zinc nitrate aluminum solutions is two, synthesis white precipitate presoma.Leave standstill and filter, filter cake sieves through deionized water drip washing, drying, grinding, calcine after obtain aluminum-doped zinc oxide nanometer powder.The method preparing aluminum-doped zinc oxide nanometer powder disclosed in the patent of publication number CN102616829A such as Qiu Fagui is: zinc nitrate, aluminum nitrate and citric acid or urea or carbohydrazide are put into beaker, wherein the mol ratio of nitrate and citric acid or urea or carbohydrazide is 0.5 ~ 1.2, aluminium content 0.5 ~ 5.0at%, add deionized water, stirring makes it fully dissolve, then be placed in continuous heating in digital display constant temperature blender with magnetic force to stir, and the temperature controlling solution is between 60 DEG C ~ 70 DEG C, until solution forms colloidal sol; The temperature of control colloidal sol, stops adding thermal agitation until form lurid gel at 80 DEG C; The beaker that gel is housed is put into the chamber type electric resistance furnace being preheating to 180 DEG C and maintains this temperature and after 3 ~ 5 hours, stop heating, treat that it naturally cools to room temperature, taking-up obtains precursor powder and the precursor powder obtained is placed in chamber type electric resistance furnace, with the ramp to 800 DEG C of 5 DEG C/min, be incubated 2 ~ 4 hours, then naturally cool to room temperature, obtain aluminium-doped zinc oxide nano material.
Said method prepares aluminum-doped zinc oxide nanometer powder complex process, and cost is higher, and granularity, dispersiveness are wayward.Therefore, be necessary to explore a kind of cost low, technique is simple, granularity controlled, the preparation method with the aluminum-doped zinc oxide nanometer powder of meso-hole structure of high dispersive.
Summary of the invention
The invention provides a kind of simple, the method that efficient, low cost prepares aluminum-doped zinc oxide nanometer powder.
Processing step of the present invention is as follows:
1, by zinc nitrate, aluminum nitrate, amine organic matter and adjuvant wiring solution-forming according to a certain percentage, wherein the mol ratio of aluminum nitrate and zinc nitrate is 0.005-0.15, the mol ratio of amine organic matter and zinc nitrate is 3-6, and the mol ratio of adjuvant and zinc nitrate is 0.1-1;
2, solution heating step 1 formed, solution evaporation, concentrated after react, obtain predecessor powder;
3, by predecessor powder in 400-800 DEG C of temperature range, under air react 1-5 hour, obtain aluminium-doped zinc oxide nanometer powder.
4, the amine organic matter described in step 1 is at least one in urea, glycine; Adjuvant is the one in glucose, citric acid, sucrose.
Advantage of the present invention is:
1, the pyrolytic reaction in liquid phase between each raw material is utilized to prepare precursor powder, simple process, quick, can complete in tens minutes
A large amount of gases of 2, releasing in each raw material reaction process can effectively prevent powder product from reuniting;
3, the interpolation of adjuvant, can reduce reaction temperature, makes reaction become gentle controlled.And in follow-up heat treatment process, serve as the effect of dispersant, stop powder to be reunited and grow up;
4, utilize liquid phase to mix each raw material, aluminum nitrate and the Homogeneous phase mixing of zinc nitrate in molecule rank can be realized, be conducive to being uniformly distributed of aluminium element in product;
5, the controlled aluminum-doped zinc oxide nanometer powder of granularity can be obtained by the proportioning and subsequent heat temperature regulating raw material;
6, prepared aluminum-doped zinc oxide nanometer powder purity is high, good dispersion and possess meso-hole structure, is adsorbed with organic pollutants efficiency high;
7, equipment is simple, and technological process is short, and efficiency is high, and cost is low, is applicable to large-scale industrial and produces.
Accompanying drawing explanation
Fig. 1 is the XRD figure of aluminum-doped zinc oxide nanometer powder of the present invention (aluminium doping is 4mol%).
Fig. 2 is the EDS figure of aluminum-doped zinc oxide nanometer powder of the present invention (aluminium doping is 4mol%).
Fig. 3 is the TEM figure of aluminum-doped zinc oxide nanometer powder of the present invention (aluminium doping is 4mol%)
Fig. 4 is the nitrogen adsorption desorption curve map of aluminum-doped zinc oxide nanometer powder of the present invention (aluminium doping is 4mol%).
Fig. 5 is the absorption property figure (1g/L adsorbent, 50ppm methyl orange pollutant) of aluminum-doped zinc oxide nanometer powder of the present invention (aluminium doping is 4mol%)
Detailed description of the invention
Embodiment 1
Take zinc nitrate 0.1 mole, aluminum nitrate 0.002 mole, 0.4 mole, urea, glucose 0.03 mole is dissolved in distilled water, is mixed with solution, is placed in by solution on controllable temperature electric furnace and heats.Solution, in experience volatilization, concentrated rear decomposition, obtains predecessor powder.By precursor powder 700 DEG C, react 1 hour in stove under air atmosphere condition, obtain the aluminium-doped zinc oxide nanometer powder with meso-hole structure.Gained powder particle size is 30 ~ 60nm, and concentration is that the methyl orange contaminant degradation of 20ppm is needed 15min by the adsorbent of 1g/L.
Embodiment 2
Take zinc nitrate 0.1 mole, aluminum nitrate 0.004 mole, 0.42 mole, urea, glucose 0.025 mole is dissolved in distilled water, is mixed with solution, is placed in by solution on controllable temperature electric furnace and heats.Solution, in experience volatilization, concentrated rear decomposition, obtains predecessor powder.By precursor powder 700 DEG C, react 1 hour in stove under air atmosphere condition, obtain the aluminium-doped zinc oxide nanometer powder with meso-hole structure.Gained powder particle size is 20 ~ 50nm, and concentration is that the methyl orange contaminant degradation of 20ppm is needed 5min by the adsorbent of 1g/L.
Embodiment 3
Take zinc nitrate 0.1 mole, aluminum nitrate 0.008 mole, 0.43 mole, urea, glucose 0.03 mole is dissolved in distilled water, is mixed with solution, is placed in by solution on controllable temperature electric furnace and heats.Solution, in experience volatilization, concentrated rear decomposition, obtains predecessor powder.By precursor powder 500 DEG C, react 1 hour in stove under air atmosphere condition, obtain the aluminium-doped zinc oxide nanometer powder with meso-hole structure.Gained powder particle size is 15 ~ 35nm, and concentration is that the methyl orange contaminant degradation of 20ppm is needed 3min by the adsorbent of 1g/L.
Embodiment 4
Take zinc nitrate 0.1 mole, aluminum nitrate 0.004 mole, 0.45 mole, urea, glucose 0.03 mole is dissolved in distilled water, is mixed with solution, is placed in by solution on controllable temperature electric furnace and heats.Solution, in experience volatilization, concentrated rear decomposition, obtains predecessor powder.By precursor powder 500 DEG C, react 1 hour in stove under air atmosphere condition, obtain the aluminium-doped zinc oxide nanometer powder with meso-hole structure.Gained powder particle size is 10 ~ 35nm, and concentration is that the methyl orange contaminant degradation of 50ppm is needed 7min by the adsorbent of 1g/L.
Claims (4)
1. a method for aluminum-doped zinc oxide nanometer powder, described method characteristic is,
(1) by zinc nitrate, aluminum nitrate, amine organic matter and adjuvant wiring solution-forming according to a certain percentage, wherein the mol ratio of aluminum nitrate and zinc nitrate is 0.005-0.15, the mol ratio of amine organic matter and zinc nitrate is 3-6, and the mol ratio of adjuvant and zinc nitrate is 0.1-1;
(2) solution is heated, solution evaporation, concentrated after react, obtain predecessor powder;
(3) by predecessor powder in 400-800 DEG C of temperature range, under air react 1-5 hour, obtain aluminium-doped zinc oxide nanometer powder.
2. the preparation method of a kind of aluminum-doped zinc oxide nanometer powder according to claim 1, is characterized in that the amine organic matter in step (1) is at least one in urea, glycine.
3. the preparation method of a kind of aluminum-doped zinc oxide nanometer powder according to claim 1, is characterized in that in step, the adjuvant described in (1) is the one in glucose, citric acid, sucrose.
4. the preparation method of a kind of aluminum-doped zinc oxide nanometer powder according to claim 1, it is characterized in that: by regulating raw material, granularity is controlled to produce proportioning, favorable dispersibility and have mesoporous mechanism, is adsorbed with the aluminium-doped zinc oxide nanometer powder that organic pollutants efficiency is high.
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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 |
| US20220040674A1 (en) * | 2020-08-07 | 2022-02-10 | Pure-Light Technologies, Inc. | Surface coatings for self-decontamination |
| US11906157B2 (en) | 2020-08-07 | 2024-02-20 | Pure-Light Te chnologies, Inc. | Photocatalyst formulations and coatings |
| 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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| US11906157B2 (en) | 2020-08-07 | 2024-02-20 | Pure-Light Te chnologies, Inc. | Photocatalyst formulations and coatings |
| 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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