CN102616828B - Nano zinc oxide-doped powder and preparation method thereof - Google Patents
Nano zinc oxide-doped powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nano zinc oxide-doped powder and a preparation method thereof. Silicon-aluminum co-doped nano zinc oxide powder is synthesized by using a co-precipitation and calcining one-step method; and the mol ratio of aluminum as a doping element to zinc oxide and the mol ratio of silicon as a doping element to the zinc oxide are (0.03:1)-(0.18:1) respectively. The nano zinc oxide-doped powder disclosed by the invention has the advantages that the whiteness of nano zinc oxide and the light transmittance in a visible light band are improved; the photocatalytic activity of the nano zinc oxide, the dissolving of zinc ions and the particle size increase of the zinc oxide particles in the roasting process are inhibited; and the dispersibility of the nano zinc oxide in water is improved; and the preparation method has the advantages of convenience in operation, simple requirement on equipment, short process flow, low cost and suitability for large-scale industrial production.
Description
Technical field
The present invention relates to a kind of nanometer Zinc oxide powder and preparation method thereof, particularly a kind of nanometer doped zinc oxide powder and preparation method thereof.
Background technology
Nano zine oxide refers to the zinc oxide material of particle diameter between 1～100nm, there is the performance better than common zinc oxide material, as non-migrating, fluorescence, piezoelectricity, absorption and scatters ultraviolet ability etc., at aspects such as magnetic, light, electricity, sensitivity, antibiotic and sterilizing, ultraviolet screeners, it is a kind of new function material had a extensive future.Yet nano zine oxide exists the color shortcomings such as Huang, bad dispersibility, the easy stripping of zine ion partially in actual use, thereby has limited its industrialized application.At present, prepare the doping zinc-oxide powder and receive much concern, the advantage such as the doping zinc-oxide powder has good dispersion property, nontoxic, whiteness is higher, physical and chemical stability is better and production cost is lower.
The preparation method of spherical aluminum-doped zinc oxide nanometer powder (country origin: China, publication number: 101665237, publication date: 2010-3-10) disclose first soluble zinc salt and aluminium salt are mixed with to mixing salt solution by a certain percentage, then add ammoniacal liquor or ammonium salt to generate precursor, precursor is moved in reactor and carry out hydro-thermal reaction again, finally 100 ℃ of oven dry, can obtain spherical aluminum-doped zinc oxide nanometer powder.The method is used the hydro-thermal reaction method, higher to equipment requirements, be difficult for large-scale industrial production, and the spherical aluminum-doped zinc oxide powder whiteness obtained is not very high.
A kind of multi-doping zinc-oxide-base wide-bandgap conducting material and preparation method thereof (country origin: China, publication number: 101661808, publication date: 2010-3-3) disclose dopant source and zinc source are prepared burden according to mole proportioning of each doped element and zinc element, then obtain forerunner's adulterated powder through mixing, oven dry and grinding, again by forerunner's adulterated powder 500 ℃～1000 ℃ pre-burnings 2～24 hours, finally, by the adulterated powder moulded section after pre-burning and 1100 ℃～1450 ℃ sintering 1～16 hour, make multi-doping zinc-oxide-base wide-bandgap conducting material.The weak point of the method mainly is: the mode of 1. mixing by ball milling is difficult to obtain uniform doping, and then affects the homogeneity of Zinc oxide-base electro-conductive material; 2. easily introduce a large amount of impurity in ball milling mixing process, cause Zinc oxide-base electro-conductive material purity drop; 3. the forerunner's adulterated powder obtained after ball milling need to carry out sintering under comparatively high temps, and under high temperature, hotchpotch and zinc oxide easily react and generates the reunion of easily growing up of segregation phase and zinc oxide particle, thereby affects its electroconductibility and dispersiveness.
Summary of the invention
Goal of the invention: for the problems referred to above, the purpose of this invention is to provide a kind of nanometer doped zinc oxide powder and preparation method thereof, improve the performance of nanometer Zinc oxide powder, and be suitable for suitability for industrialized production.
Technical scheme: a kind of nanometer doped zinc oxide powder, doped element is aluminium and silicon, described doped element aluminium, described doped element silicon is 0.03: 1 with the mol ratio of zinc oxide separately～and 0.18: 1.
The preparation method of above-mentioned a kind of nanometer doped zinc oxide powder, the method comprises the following steps:
(1) aluminium salt and zinc salt are dissolved in deionized water to the mixing salt solution that forms 0.2～2 mol/L jointly;
(2) temperature of regulating above-mentioned mixing salt solution is 30 ℃～60 ℃, the precipitant solution that adds while stirring 0.2～3 mol/L, when the pH of system value reaches 3.5～4.0, suspend and to add precipitant solution, to the aqueous silicate solution that adds 0.1～1 mol/L in coprecipitated product, after aqueous silicate solution adds, continue to add the precipitant solution of 0.2～3 mol/L, regulation system pH value is 6.5～8.5, is warming up to 70 ℃～90 ℃, continues to stir slaking 0.5～4h;
(3) above-mentioned coprecipitated product is filtered, remove soluble salt with the deionized water repetitive scrubbing, when the specific conductivity of filtrate≤260 μ S/cm, finish washing, drying obtains white product, white product is calcined to 1～5h under 700 ℃～900 ℃, obtain the nanometer Zinc oxide powder of sial codoped after pulverizing.
Aluminium salt described in step (1) be Tai-Ace S 150, aluminum nitrate, aluminum chloride one of them, described zinc salt be zinc sulfate, zinc nitrate, zinc chloride, zinc acetate one of them.
Aluminum ion described in step (1) in aluminium salt and the mol ratio of the zine ion in described zinc salt are 0.03: 1～0.18: 1.
Precipitant solution described in step (2) is one of them the aqueous solution of bicarbonate of ammonia, volatile salt, sodium carbonate, sodium bicarbonate, ammoniacal liquor.
Described in step (2), silicate is water glass or potassium silicate.
Silicon ion described in step (2) in silicate and the mol ratio of zinc oxide are 0.03: 1～0.18: 1.
Beneficial effect: compared with prior art, advantage of the present invention is:
1, utilize the nanometer Zinc oxide powder of co-precipitation-calcining single stage method synthesizing Si-Al codoped, the adulterated al element has improved the nano zine oxide whiteness on the one hand, improve on the other hand the light transmission of nano zine oxide at visible light wave range, for adapting to the different application field, provide precondition;
2, silicate, simultaneously as silicon source and precipitation agent, has reduced the pollution to environment when having saved cost; The doped silicon element has suppressed again the stripping of zine ion when having suppressed the photocatalytic activity of nano zine oxide, improved the dispersiveness of nano zine oxide in water, suppressed zinc oxide particle diameter in roasting process grows up simultaneously, alleviated between particle and reunited to a certain extent, made the powder dispersity that finally makes good and stable;
3, the nanometer Zinc oxide powder that the inventive method is prepared has light stability and the transparency is excellent, the zine ion stripping quantity is little, particle diameter is little and the advantages such as homogeneous, good dispersity;
4, the inventive method is easy to operate, equipment requirements is simple, technical process is short, cost is low, is applicable to large-scale industrial production.
Embodiment
Below in conjunction with specific embodiment, further illustrate the present invention, should understand these embodiment only is not used in and limits the scope of the invention for the present invention is described, after having read the present invention, those skilled in the art all fall within the application's claims limited range to the modification of the various equivalent form of values of the present invention.
Embodiment 1: by the ZnSO of 28.76g
47H
20 and the Al of 6.66g
2(SO4)
318H
20 adds the mixing salt solution that in deionized water, the formation total concn is 1.0 mol/L.The temperature of controlling mixing salt solution is 50 ℃, while stirring to the ammonium bicarbonate soln that adds 1.5 mol/L in mixing salt solution, when the pH of system value reaches 3.8, suspend and to add ammonium bicarbonate soln, to 24 milliliters of the sodium silicate aqueous solutions that adds 0.5 mol/L in coprecipitated product, after sodium silicate aqueous solution adds, continue to add the ammonium bicarbonate soln of 1.5 mol/L, the pH value of regulation system is 7.5, is warming up to 75 ℃, stirs slaking 2h.The coprecipitated product of gained is filtered, remove soluble salt with the deionized water repetitive scrubbing, when the specific conductivity of filtrate is 200 μ S/cm, finish washing, drying obtains white product, and white product is calcined to 2h under 800 ℃, obtains the nanometer Zinc oxide powder of sial codoped after pulverizing.In product, the mol ratio of doped element aluminium and zinc oxide is 0.1: 1, and the mol ratio of doped element silicon and zinc oxide is 0.12: 1, and the whiteness that records product is 91, and median size is 23nm.
Embodiment 2: by the ZnSO of 28.76g
47H
20 and the Al of 1.998g
2(SO4)
318H
20 adds the mixing salt solution that in deionized water, the formation total concn is 0.2 mol/L.The temperature of controlling mixing salt solution is 30 ℃, while stirring to the sal volatile that adds 3 mol/L in mixing salt solution, when the pH of system value reaches 3.5, suspend and to add sal volatile, to 18 milliliters of the potassium silicate aqueous solutions that adds 1.0 mol/L in coprecipitated product, after potassium silicate aqueous solution adds, continue to add the sal volatile of 3.0 mol/L, the pH value of regulation system is 7.0, is warming up to 90 ℃, stirs slaking 0.5h.The coprecipitated product of gained is filtered, remove soluble salt with the deionized water repetitive scrubbing, when the specific conductivity of filtrate is 260 μ S/cm, finish washing, drying obtains white product, and white product is calcined to 5h under 700 ℃, obtains the nanometer Zinc oxide powder of sial codoped after pulverizing.In product, the mol ratio of doped element aluminium and zinc oxide is 0.03: 1, and the mol ratio of doped element silicon and zinc oxide is 0.18: 1, and the whiteness that records product is 90, and median size is 17nm.
Embodiment 3: by the Zn(NO of 29.75g
3)
26H
2the Al(NO of O and 6.75g
3)
39H
20 adds the mixing salt solution that in deionized water, the formation total concn is 2.0 mol/L.The temperature of controlling mixing salt solution is 60 ℃, while stirring to the sodium carbonate solution that adds 0.2 mol/L in mixing salt solution, when the pH of system value reaches 4.0, suspend and to add sodium carbonate solution, to 30 milliliters of the sodium silicate aqueous solutions that adds 0.1 mol/L in coprecipitated product, after sodium silicate aqueous solution adds, continue to add the sodium carbonate solution of 0.2 mol/L, the pH value of regulation system is 8.0, is warming up to 70 ℃, stirs slaking 4h.The coprecipitated product of gained is filtered, remove soluble salt with the deionized water repetitive scrubbing, when the specific conductivity of filtrate is 150 μ S/cm, finish washing, drying obtains white product, and white product is calcined to 1h under 900 ℃, obtains the nanometer Zinc oxide powder of sial codoped after pulverizing.In product, the mol ratio of doped element aluminium and zinc oxide is 0.18: 1, and the mol ratio of doped element silicon and zinc oxide is 0.03: 1, and the whiteness that records product is 94, and median size is 29nm.
Embodiment 4: by the ZnCl of 13.6g
2alCl with 1.064g
3add in deionized water and form the mixing salt solution that total concn is 0.8 mol/L.The temperature of controlling mixing salt solution is 38 ℃, while stirring to the sodium hydrogen carbonate solution that adds 2.0 mol/L in mixing salt solution, when the pH of system value reaches 3.6, suspend and to add sodium hydrogen carbonate solution, to 50 milliliters of the potassium silicate aqueous solutions that adds 0.3 mol/L in coprecipitated product, after potassium silicate aqueous solution adds, continue to add the sodium hydrogen carbonate solution of 2.0 mol/L, the pH value of regulation system is 8.5, is warming up to 80 ℃, stirs slaking 1h.The coprecipitated product of gained is filtered, remove soluble salt with the deionized water repetitive scrubbing, when the specific conductivity of filtrate is 180 μ S/cm, finish washing, drying obtains white product, and white product is calcined to 4h under 750 ℃, obtains the nanometer Zinc oxide powder of sial codoped after pulverizing.In product, the mol ratio of doped element aluminium and zinc oxide is 0.08: 1, and the mol ratio of doped element silicon and zinc oxide is 0.15: 1, and the whiteness that records product is 92, and median size is 20nm.
Embodiment 5: by (the CH of 21.95g
3cOO)
2zn2H
20 and the Al of 9.324g
2(SO
4)
318H
20 adds the mixing salt solution that in deionized water, the formation total concn is 1.5 mol/L.The temperature of controlling mixing salt solution is 55 ℃, while stirring to the ammoniacal liquor that adds 1.0 mol/L in mixing salt solution, when the pH of system value reaches 3.9, suspend and to add ammoniacal liquor, to 8.75 milliliters of the sodium silicate aqueous solutions that adds 0.8 mol/L in coprecipitated product, after sodium silicate aqueous solution adds, continue to add the ammoniacal liquor of 1.0 mol/L, the pH value of regulation system is 6.5, is warming up to 85 ℃, stirs slaking 3h.The coprecipitated product of gained is filtered, remove soluble salt with the deionized water repetitive scrubbing, when the specific conductivity of filtrate is 220 μ S/cm, finish washing, drying obtains white product, and white product is calcined to 3h under 850 ℃, obtains the nanometer Zinc oxide powder of sial codoped after pulverizing.In product, the mol ratio of doped element aluminium and zinc oxide is 0.14: 1, and the mol ratio of doped element silicon and zinc oxide is 0.07: 1, and the whiteness that records product is 93, and median size is 26nm.
To following 3 comparative examples and above-mentioned 5 embodiment, analyze by experiment contrast the present invention and adulterated the nanometer Zinc oxide powder of silicon and aluminium in photocatalytic activity, zine ion stripping, dispersed advantage simultaneously.
Comparative example 1: by the ZnSO of 28.76g
47H
20 adds the zinc solution that in deionized water, formation concentration is 1.0 mol/L, the temperature of controlling zinc solution is 50 ℃, while stir to the ammonium bicarbonate soln that adds 1.5 mol/L in zinc solution, the pH value of regulation system is 7.5, be warming up to 75 ℃, stir slaking 2h.The coprecipitated product of gained is filtered, remove soluble salt with the deionized water repetitive scrubbing, when the specific conductivity of filtrate is 200 μ S/cm, finish washing, drying obtains white product, and white product is calcined to 2h under 800 ℃, obtains pure micron Zinc oxide powder after pulverizing.The whiteness that records pure micron Zinc oxide powder is 80, and median size is 210nm.
Comparative example 2: by the ZnSO of 28.76g
47H
20 and the Al of 6.66g
2(SO4)
318H
20 adds the mixing salt solution that in deionized water, the formation total concn is 1.0 mol/L.The temperature of controlling mixing salt solution is 50 ℃, stirs on one side to the ammonium bicarbonate soln that adds 1.5 mol/L in mixing salt solution, and the pH value of regulation system is 7.5, is warming up to 75 ℃, stirring slaking 2h.The coprecipitated product of gained is filtered, remove soluble salt with the deionized water repetitive scrubbing, when the specific conductivity of filtrate is 200 μ S/cm, finish washing, drying obtains white product, and white product is calcined to 2h under 800 ℃, obtains the micron Zinc oxide powder of aluminium doping after pulverizing.In the micron Zinc oxide powder of aluminium doping, the mol ratio of doped element aluminium and zinc oxide is 0.1: 1, and the whiteness that records the micron Zinc oxide powder of aluminium doping is 88, and median size is 145nm.
Comparative example 3: by the ZnSO of 28.76g
47H
20 adds the zinc solution that in deionized water, formation concentration is 1.0 mol/L, the temperature of controlling zinc solution is 50 ℃, while stirring to 24 milliliters of the sodium silicate aqueous solutions that adds 0.5 mol/L in zinc solution, after sodium silicate aqueous solution adds, the ammonium bicarbonate soln that adds 1.5 mol/L, the pH value of regulation system is 7.5, is warming up to 75 ℃, stirs slaking 2h.The coprecipitated product of gained is filtered, remove soluble salt with the deionized water repetitive scrubbing, when the specific conductivity of filtrate is 200 μ S/cm, finish washing, drying obtains white product, and white product is calcined to 2h under 800 ℃, obtains the micron Zinc oxide powder of silicon doping after pulverizing.In the micron Zinc oxide powder of silicon doping, the mol ratio of doped element silicon and zinc oxide is 0.12: 1, and the whiteness that records the micron Zinc oxide powder of silicon doping is 85, and median size is 121nm.
The determination experiment of Zinc oxide powder photocatalytic activity: in XPA photochemical reaction instrument, add the standby Zinc oxide powder of 1.0 restraints, add again the methyl orange solution that 500 milliliters of mass concentrations are 20 mg/litre, open the air that stirs and pass into 0.02 liter/min of flow from bottom, open ultraviolet lamp, power 20W, wavelength 254nm, after one period reaction times, sampling is 15 milliliters, and centrifugation, get supernatant liquid and tested.Measure the absorbancy of solution under its maximum absorption wavelength by spectrophotometer, degradation rate is calculated as follows:
In formula, η is degradation rate (%); A
0, A
tbefore being respectively degraded, the solution absorbance of t after the time; C
0, C
tbefore being respectively degraded, the strength of solution of t after the time.
In light-catalyzed reaction, after 120 minutes, the different Zinc oxide powders of embodiment 1～embodiment 5, comparative example 1～comparative example 3 are as shown in the table to the degradation rate of tropeolin-D:
As can be seen here, embodiment 1～embodiment 5 is that simultaneously the adulterated photocatalytic activity of nanometer Zinc oxide powder of silicon and aluminium of the present invention is effectively suppressed.
The determination experiment of Zinc oxide powder zine ion stripping: Zinc oxide powder is added respectively in ammoniacal liquor that deionized water, quality percentage composition are 1%, salpeter solution that the quality percentage composition is 0.01%, be mixed with the suspension that solid content is 5%, under 30 ℃, stir 240 minutes, high speed centrifugation separates, and the zinc ion concentration of measuring in the stillness of night with Vista-AX type plasma emission spectrum is as shown in the table:
As can be seen here, embodiment 1～embodiment 5 is that simultaneously the adulterated zine ion stripping concentration of nanometer Zinc oxide powder of silicon and aluminium of the present invention obviously reduces.
The determination experiment of Zinc oxide powder dispersiveness: get the 10g Zinc oxide powder and the 0.3g Sodium hexametaphosphate 99 adds in deionized water, with the ultrasonic dispersion of JYD650 Intelligent supersonic cell pulverization 0.5 hour, be mixed with the slurry that the quality percentage composition is 5%, pack into the graduated test tube of diameter 1.5cm, total length 15cm, vertically be placed on test-tube stand, standing 2 days at normal temperatures, the settling height of observing zinc oxide was as shown in the table:
As can be seen here, embodiment 1～embodiment 5 is that simultaneously the adulterated dispersiveness of nanometer Zinc oxide powder of silicon and aluminium of the present invention obviously improves.
Claims (7)
1. a nanometer doped zinc oxide powder, it is characterized in that: doped element is aluminium and silicon, described doped element aluminium, described doped element silicon is 0.03: 1 with the mol ratio of zinc oxide separately～and 0.18: 1.
2. the preparation method of a kind of nanometer doped zinc oxide powder according to claim 1 is characterized in that the method comprises the following steps:
(1) aluminium salt and zinc salt are dissolved in deionized water to the mixing salt solution that forms 0.2～2 mol/L jointly;
(2) temperature of regulating above-mentioned mixing salt solution is 30 ℃～60 ℃, the precipitant solution that adds while stirring 0.2～3 mol/L, when the pH of system value reaches 3.5～4.0, suspend and to add precipitant solution, to the aqueous silicate solution that adds 0.1～1 mol/L in coprecipitated product, after aqueous silicate solution adds, continue to add the precipitant solution of 0.2～3 mol/L, regulation system pH value is 6.5～8.5, is warming up to 70 ℃～90 ℃, continues to stir slaking 0.5～4h;
(3) above-mentioned coprecipitated product is filtered, remove soluble salt with the deionized water repetitive scrubbing, when the specific conductivity of filtrate≤260 μ S/cm, finish washing, drying obtains white product, white product is calcined to 1～5h under 700 ℃～900 ℃, obtain the nanometer Zinc oxide powder of sial codoped after pulverizing.
3. the preparation method of a kind of nanometer doped zinc oxide powder according to claim 2, it is characterized in that: aluminium salt described in step (1) be Tai-Ace S 150, aluminum nitrate, aluminum chloride one of them, described zinc salt be zinc sulfate, zinc nitrate, zinc chloride, zinc acetate one of them.
4. the preparation method of a kind of nanometer doped zinc oxide powder according to claim 2, it is characterized in that: the aluminum ion described in step (1) in aluminium salt and the mol ratio of the zine ion in described zinc salt are 0.03: 1～0.18: 1.
5. the preparation method of a kind of nanometer doped zinc oxide powder according to claim 2 is characterized in that: precipitant solution described in step (2) is one of them the aqueous solution of bicarbonate of ammonia, volatile salt, sodium carbonate, sodium bicarbonate, ammoniacal liquor.
6. the preparation method of a kind of nanometer doped zinc oxide powder according to claim 2, it is characterized in that: described in step (2), silicate is water glass or potassium silicate.
7. the preparation method of a kind of nanometer doped zinc oxide powder according to claim 2, it is characterized in that: the silicon ion described in step (2) in silicate and the mol ratio of zinc oxide are 0.03: 1～0.18: 1.
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| CN102923758B (en) * | 2012-11-27 | 2015-03-18 | 中国科学院广州能源研究所 | Preparation method of highly-aluminium-doped zinc oxide nano-powder |
| CN103570056B (en) * | 2013-11-22 | 2015-01-07 | 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 |
| CN104445372B (en) * | 2014-11-26 | 2016-03-02 | 燕山大学 | A kind of method preparing carbon doping Zinc oxide nanoparticle |
| CN105197980A (en) * | 2015-07-16 | 2015-12-30 | 南京工业大学 | Preparation method of silicon and zirconium co-doped zinc oxide nano powder |
| WO2017208522A1 (en) * | 2016-06-02 | 2017-12-07 | エム・テクニック株式会社 | Ultraviolet and/or near-infrared blocking agent composition for transparent material |
| CN106430284A (en) * | 2016-09-13 | 2017-02-22 | 苏州市泽镁新材料科技有限公司 | Preparation method of sulfur-doped zinc oxide nano material |
| CN107892323A (en) * | 2017-11-02 | 2018-04-10 | 畅的新材料科技（上海）有限公司 | A kind of preparation method of Al doping ZnO low-resistivity nano-powders |
| CN109235056A (en) * | 2018-10-30 | 2019-01-18 | 广东菲安妮皮具股份有限公司 | A kind of preparation method for PVC artificial leather mould inhibitor |
| CN111393889B (en) * | 2020-04-17 | 2021-11-30 | 肇庆市盛浩新材料科技有限公司 | Anticorrosive and mildewproof material for paint and preparation method and application thereof |
| GB202206338D0 (en) * | 2022-04-29 | 2022-06-15 | Johnson Matthey Plc | Stabilised zinc oxide materials |
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