CN107129294A - A kind of preparation method for mixing the high agglutinating property zinc oxide nano-powder of aluminium - Google Patents
A kind of preparation method for mixing the high agglutinating property zinc oxide nano-powder of aluminium Download PDFInfo
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The present invention discloses a kind of preparation method for mixing the high agglutinating property zinc oxide nano-powder of aluminium, comprises the following steps：Surface modification agent solution is prepared, Zn (NO are added in surface modification agent solution3)2·6H2O and Al (NO3)3·9H2O, adds urea, is uniformly mixed；Heating, reacts more than 2h, obtains white precipitate under agitation；Mother liquor continues to stir and be aged through ultrasonication；Vacuum filtration, products therefrom is washed twice with weak aqua ammonia, then uses organic solvent washing；It is dried in vacuo after washing, AZO presomas are made in ground, sieving；AZO presomas are calcined, high agglutinating property Al-Doped ZnO nano-powder is produced.The present invention uses chemical coprecipitation, add a certain amount of coating material, the hard aggregation between powder can be efficiently reduced by adding coating material, and with reference to ultrasonication technological means, smaller size, good dispersion, the Al-Doped ZnO nano-powder of uniform particle sizes is prepared.
Description
Technical field
The present invention relates to zinc oxide target preparing technical field, more particularly to one kind mixes the high agglutinating property zinc oxide nano of aluminium
The preparation method of body.
Background technology
Zinc oxide (ZnO) is a kind of semi-conducting material, and its raw material is cheap, nontoxic, in surface acoustic wave device, flat
The fields such as panel display, solar cell, building glass are applied., can be by nano zine oxide table in polymer application
Face is modified to be added as additive, so that there is polymer the function such as uvioresistant, sterilization to be adulterated after Al elements, can
To improve free carrier concentration in ZnO, its light to region of ultra-red is set to produce stronger absorption and reflection.It is prepared into
Nano-particle.And be applied in polymer, it is used as the transparent heat-insulated addition such as ITO (tin indium oxide) and ATO (tin-antiomony oxide)
The substitute of agent, can be greatly lowered production cost, with very big realistic meaning.
The preparation method of zinc oxide (AZO) nano-particle mainly have chemical coprecipitation, microemulsion method, hydro-thermal method, colloidal sol-
Gel method etc..Using diameter of particle made from micro emulsion method is small and narrowly distributing, but cost is high, yield poorly, it is difficult to industrially industry
Change；Hydro-thermal method prepares powder amount of investment greatly, and the purity of powder is difficult to control during production in enormous quantities；Sol-gal process is to ingredient requirement
It is high, it is difficult to meet industrial production demand.Comparatively speaking, adulterated powder is produced using chemical coprecipitation, up to atom
The uniformity of level, meanwhile, cost is low, yield is big, but to obtain powder hard aggregation more serious for the legal system, and particle diameter distribution is wider.
The content of the invention
The present invention uses surface modification method there is provided a kind of preparation method for mixing the high agglutinating property zinc oxide nano-powder of aluminium,
Solve that Al-Doped ZnO nano-powder hard aggregation prepared by existing chemical coprecipitation is more serious and particle diameter distribution is wider asks
Topic.
In order to solve the above technical problems, the technical scheme is that：
A kind of preparation method for mixing the high agglutinating property zinc oxide nano-powder of aluminium, comprises the following steps：
(1) compound concentration is 15~20g/L surface modification agent solution, and Zn is added in surface modification agent solution
(NO3)2·6H2O and Al (NO3)3·9H2O, the urea of addition excessive more than 20%, is uniformly mixed；
(2) 80~95 DEG C are progressively warming up to, more than 2h is reacted under agitation, white precipitate is obtained；
(3) mother liquor continues to stir and be aged 1~24 hour after ultrasonication 1 hour；
(4) it is filtered by vacuum, products therefrom is washed twice with 0.1mol/L weak aqua ammonias, then uses organic solvent washing；
(5) it is dried in vacuo after washing, AZO presomas are made in ground, sieving；
(6) 3~5 DEG C/min of AZO presomas is warming up to 100~200 DEG C, is incubated 30~50min, then with 3 DEG C/min liters
Temperature is incubated 3~5 hours, produces Al-Doped ZnO nano-powder to 600~800 DEG C.
Wherein it is preferred to, the Al and the Zn atomic percent are 3~5%.
Wherein it is preferred to, the coating material is times in soluble starch, polyethylene glycol and dodecyl sodium sulfate
Meaning is one or more of.
Wherein it is preferred to, addition and the Zn (NO of the coating material3)2·6H2O weight ratio is 1：15~20.
Wherein it is preferred to, the frequency range of ultrasonically treated ultrasonic wave is 40~60MHz in the step (3).
Wherein it is preferred to, the organic solvent in the step (4) is that volume ratio is 1：3：5 ethanol, ethyl acetate and ring
Hexanol.
Beneficial effects of the present invention：
The present invention uses chemical coprecipitation, adds a certain amount of coating material, is controlled by coating material
The dispersity and size distribution of sediment, intergranular hard aggregation is reduced in conjunction with ultrasonication technology during co-precipitation,
Make the distribution of particles of sediment more uniform.It is successfully prepared spherical, good dispersion, the nanometer Al-Doped ZnO of uniform particle sizes
Powder.Analytical structure shows that Al ions have successfully been doped in zinc oxide lattice, keeps ZnO hexagonal wurtzite structure.Pass through
SEM is observed, and it is~100nm to show obtained Al-Doped ZnO particle diameter of nanometer powder, and particle diameter distribution is uniform,
Interface is clear between grain, good fluidity.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, without having to pay creative labor, may be used also
To obtain other accompanying drawings according to these accompanying drawings.
Fig. 1 is to mix the typical microstructure figure of the high agglutinating property zinc oxide nano-powder of aluminium in the embodiment of the present invention 1.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based in the present invention
Embodiment, all other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1
The present embodiment provides a kind of preparation method for mixing the high agglutinating property zinc oxide nano-powder of aluminium, comprises the following steps：
(1) compound concentration is 18g/L soluble starch solution, is added in soluble starch solution
Zn(NO3)2·6H2O and Al (NO3)3·9H2O, the urea of addition excessive more than 20%, is uniformly mixed；It is described
Al and the Zn atomic percent are 4%；The addition of the soluble starch and Zn (NO3)2·6H2O weight ratio is 1：
18；
(2) 90 DEG C are progressively warming up to, more than 2h is reacted under agitation, white precipitate is obtained；
(3) mother liquor is after ultrasonication 1 hour, and the frequency range of ultrasonic wave is 40~60MHz, continues to stir and be aged
12 hours；
(4) it is filtered by vacuum, products therefrom is washed twice with 0.1mol/L weak aqua ammonias, then uses organic solvent washing；It is organic molten
Agent is that volume ratio is 1：3：5 ethanol, ethyl acetate and cyclohexanol；
(5) it is dried in vacuo after washing, AZO presomas are made in ground, sieving；
(6) 3~5 DEG C/min of AZO presomas is warming up to 150 DEG C, is incubated 40min, then 700 DEG C are warming up to 3 DEG C/min,
Insulation 4 hours, produces Al-Doped ZnO nano-powder.
Observed (as shown in Figure 1) by SEM, it can be seen that Al-Doped ZnO nanometer produced by the present invention
Powder average grain diameter is 100nm, and particle diameter distribution is uniform, and interface is clear between particle, good dispersion.
Embodiment 2
The present embodiment provides a kind of preparation method for mixing the high agglutinating property zinc oxide nano-powder of aluminium, comprises the following steps：
(1) compound concentration is 15g/L polyglycol solution, is added in polyglycol solution
Zn(NO3)2·6H2O and Al (NO3)3·9H2O, the urea of addition excessive more than 20%, is uniformly mixed；It is described
Al and the Zn atomic percent are 5%；The addition of the polyethylene glycol and Zn (NO3)2·6H2O weight ratio is 1：
15；
(2) 95 DEG C are progressively warming up to, more than 2h is reacted under agitation, white precipitate is obtained；
(3) mother liquor is after ultrasonication 1 hour, and the frequency range of ultrasonic wave is 40~60MHz, continues to stir and be aged
1 hour；
(4) it is filtered by vacuum, products therefrom is washed twice with 0.1mol/L weak aqua ammonias, then uses organic solvent washing；It is organic molten
Agent is that volume ratio is 1：3：5 ethanol, ethyl acetate and cyclohexanol；
(5) it is dried in vacuo after washing, AZO presomas are made in ground, sieving；
(6) 3~5 DEG C/min of AZO presomas is warming up to 200 DEG C, is incubated 30min, then 600 DEG C are warming up to 3 DEG C/min,
Insulation 5 hours, produces Al-Doped ZnO nano-powder.
Observed by SEM, it can be seen that Al-Doped ZnO nano-powder average grain diameter produced by the present invention
For 85nm, uniformly, interface is clear between particle, good dispersion for particle diameter distribution.
Embodiment 3
The present embodiment provides a kind of preparation method for mixing the high agglutinating property zinc oxide nano-powder of aluminium, comprises the following steps：
(1) compound concentration is 20g/L sodium dodecyl sulfate solution, and Zn is added in sodium dodecyl sulfate solution
(NO3)2·6H2O and Al (NO3)3·9H2O, the urea of addition excessive more than 20%, is uniformly mixed；The Al and Zn
Atomic percent be 3%；The addition of the dressing agent and Zn (NO3)2·6H2O weight ratio is 1：20；
(2) 80 DEG C are progressively warming up to, more than 2h is reacted under agitation, white precipitate is obtained；
(3) mother liquor is after ultrasonication 1 hour, and the frequency range of ultrasonic wave is 40~60MHz, continues to stir and be aged
24 hours；
(4) it is filtered by vacuum, products therefrom is washed twice with 0.1mol/L weak aqua ammonias, then uses organic solvent washing；It is organic molten
Agent is that volume ratio is 1：3：5 ethanol, ethyl acetate and cyclohexanol；
(5) it is dried in vacuo after washing, AZO presomas are made in ground, sieving；
(6) 3~5 DEG C/min of AZO presomas is warming up to 100 DEG C, is incubated 50min, then 800 DEG C are warming up to 3 DEG C/min,
Insulation 3 hours, produces Al-Doped ZnO nano-powder.
Observed by SEM, it can be seen that Al-Doped ZnO nano-powder average grain diameter produced by the present invention
For 125nm, uniformly, interface is clear between particle, good dispersion for particle diameter distribution.
Embodiment 4
The present embodiment provides a kind of preparation method for mixing the high agglutinating property zinc oxide nano-powder of aluminium, comprises the following steps：
(1) compound concentration is 16g/L polyglycol solution, is added in polyglycol solution
Zn(NO3)2·6H2O and Al (NO3)3·9H2O, the urea of addition excessive more than 20%, is uniformly mixed；It is described
Al and the Zn atomic percent are 3.5%；The addition of the polyethylene glycol and Zn (NO3)2·6H2O weight ratio is 1：
18；
(2) 85 DEG C are progressively warming up to, more than 2h is reacted under agitation, white precipitate is obtained；
(3) mother liquor is after ultrasonication 1 hour, and the frequency range of ultrasonic wave is 40~60MHz, continues to stir and be aged
10 hours；
(4) it is filtered by vacuum, products therefrom is washed twice with 0.1mol/L weak aqua ammonias, then uses organic solvent washing；It is organic molten
Agent is that volume ratio is 1：3：5 ethanol, ethyl acetate and cyclohexanol；
(5) it is dried in vacuo after washing, AZO presomas are made in ground, sieving；
(6) 3~5 DEG C/min of AZO presomas is warming up to 180 DEG C, is incubated 35min, then 750 DEG C are warming up to 3 DEG C/min,
Insulation 4 hours, produces Al-Doped ZnO nano-powder.
Observed by SEM, it can be seen that Al-Doped ZnO nano-powder average grain diameter produced by the present invention
For 115nm, uniformly, interface is clear between particle, good dispersion for particle diameter distribution.
Embodiment 5
The present embodiment provides a kind of preparation method for mixing the high agglutinating property zinc oxide nano-powder of aluminium, comprises the following steps：
(1) compound concentration is 18g/L sodium dodecyl sulfate solution, is added in sodium dodecyl sulfate solution
Zn(NO3)2·6H2O and Al (NO3)3·9H2O, the urea of addition excessive more than 20%, is uniformly mixed；It is described
Al and the Zn atomic percent are 4.5%；The addition of the dodecyl sodium sulfate and Zn (NO3)2·6H2O weight
Than for 1：19；The coating material is that weight ratio is 1：3 polyethylene glycol and dodecyl sodium sulfate；
(2) 83 DEG C are progressively warming up to, more than 2h is reacted under agitation, white precipitate is obtained；
(3) mother liquor is after ultrasonication 1 hour, and the frequency range of ultrasonic wave is 40~60MHz, continues to stir and be aged
20 hours；
(4) it is filtered by vacuum, products therefrom is washed twice with 0.1mol/L weak aqua ammonias, then uses organic solvent washing；It is organic molten
Agent is that volume ratio is 1：3：5 ethanol, ethyl acetate and cyclohexanol；
(5) it is dried in vacuo after washing, AZO presomas are made in ground, sieving；
(6) 3~5 DEG C/min of AZO presomas is warming up to 120 DEG C, is incubated 45min, then 650 DEG C are warming up to 3 DEG C/min,
Insulation 4 hours, produces Al-Doped ZnO nano-powder.
Observed by SEM, it can be seen that Al-Doped ZnO nano-powder average grain diameter produced by the present invention
For 92nm, uniformly, interface is clear between particle, good dispersion for particle diameter distribution.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God is with principle, and any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (6)
1. a kind of preparation method for mixing the high agglutinating property zinc oxide nano-powder of aluminium, it is characterised in that comprise the following steps：
(1) compound concentration is 15~20g/L surface modification agent solution, and Zn (NO are added in surface modification agent solution3)2·
6H2O and Al (NO3)3·9H2O, the urea of addition excessive more than 20%, is uniformly mixed；
(2) 90~100 DEG C are progressively warming up to, more than 2h is reacted under agitation, white precipitate is obtained；
(3) mother liquor continues to stir and be aged 1~24 hour after ultrasonication 1 hour；
(4) it is filtered by vacuum, products therefrom is washed twice with 0.1mol/L weak aqua ammonias, then uses organic solvent washing；
(5) it is dried in vacuo after washing, AZO presomas are made in ground, sieving；
(6) 3~5 DEG C/min of AZO presomas is warming up to 100~200 DEG C, is incubated 30~50min, then be warming up to 3 DEG C/min
600~800 DEG C, 3~5 hours are incubated, Al-Doped ZnO nano-powder is produced.
2. a kind of preparation method for mixing the high agglutinating property zinc oxide nano-powder of aluminium according to claim 1, it is characterised in that：
The Al and the Zn atomic percent are 3~5%.
3. a kind of preparation method for mixing the high agglutinating property zinc oxide nano-powder of aluminium according to claim 1, it is characterised in that：
The dressing agent is any one or a few in soluble starch, polyethylene glycol and dodecyl sodium sulfate.
4. a kind of preparation method for mixing the high agglutinating property zinc oxide nano-powder of aluminium according to claim 3, it is characterised in that：
The addition of the dressing agent and Zn (NO3)2·6H2O weight ratio is 1：15~20.
5. a kind of preparation method for mixing the high agglutinating property zinc oxide nano-powder of aluminium according to claim 1, it is characterised in that：
The frequency range of ultrasonically treated ultrasonic wave is 40~60MHz in the step (3).
6. a kind of preparation method for mixing the high agglutinating property zinc oxide nano-powder of aluminium according to claim 1, it is characterised in that：
Organic solvent in the step (4) is that volume ratio is 1：3：5 ethanol, ethyl acetate and cyclohexanol.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| CN101274775A (en) * | 2008-05-21 | 2008-10-01 | 中国科学院长春应用化学研究所 | High-conductivity aluminum-doping zinc oxide nanometer noodles powder and preparation thereof |
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- 2017-04-24 CN CN201710272666.6A patent/CN107129294A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101274775A (en) * | 2008-05-21 | 2008-10-01 | 中国科学院长春应用化学研究所 | High-conductivity aluminum-doping zinc oxide nanometer noodles powder and preparation thereof |
| CN103395826A (en) * | 2013-08-06 | 2013-11-20 | 大连交通大学 | Preparation method of aluminum doped zinc oxide nano powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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Application publication date: 20170905 |