CN107010939A - A kind of preparation method of high densification Al-Doped ZnO target - Google Patents
A kind of preparation method of high densification Al-Doped ZnO target Download PDFInfo
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- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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Abstract
The present invention discloses a kind of preparation method of high densification Al-Doped ZnO target, 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, it is compressing after mist projection granulating, biscuit is obtained, biscuit is sintered, high-compactness Al-Doped ZnO target is produced.The present invention can prepare the tiny AZO targets of high-purity, high density, grain size, and the simple controllable, production cost of manufacturing process of the present invention is low, it is easy to accomplish large-scale production.
Description
Technical field
The present invention relates to zinc oxide target preparing technical field, more particularly to a kind of high densification Al-Doped ZnO target
Preparation method.
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 reuniting more serious for the legal system, and particle diameter distribution is wider.
The content of the invention
The present invention produces the oxide powder and zinc of the aluminium doping of high dispersancy nano size using surface modification technology
Body, through granulating and forming with sintering obtain high densification AZO targets (>99.0%).This invention is due to using improvement
Chemical coprecipitation method production powder so that the preparation technology of target is simple, cost is low, be easy to industrialization.
The technical scheme is that：
A kind of preparation method of high densification Al-Doped ZnO target, 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 to 600~800 DEG C, compressing after mist projection granulating, obtains biscuit；
(7) biscuit is sintered, the sintering condition is：1200 DEG C~1400 DEG C are warming up to 2 DEG C/min, and is incubated
1~5 hour, finally cool to room temperature with the furnace, produce high-compactness Al-Doped ZnO target.
Wherein it is preferred to, the Al and the Zn atomic percent are 3~5%.
Wherein it is preferred to, the dressing agent is any one in soluble starch, polyethylene glycol and dodecyl sodium sulfate
Plant or several.
Wherein it is preferred to, addition and the Zn (NO of the dressing agent3)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.
Wherein it is preferred to, the compressing condition of the step (6) is：Pressure 100MPa~200MPa, dwell time
8min~15min.
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.
The high dispersancy nano AZO powders prepared in the process of the present invention are raw material, greatly reduce sintering temperature, favorably
In energy-saving, industrial production cost is reduced, simultaneously because sintering temperature and low make it that the AZO target crystalline grains sizes of production are small, is carried
High target mechanical strength, enhances thermal shock resistance of the target in sputter procedure.
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 the typical microstructure figure of Al-Doped ZnO powder in the embodiment of the present invention 1；
Fig. 2 is the typical microstructure figure of AZO targets 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 of high densification Al-Doped ZnO target, 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) 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
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, it is compressing after mist projection granulating, obtain biscuit；Compressing condition is：Pressure 100MPa, dwell time
12min；
(7) biscuit is sintered, the sintering condition is：1200 DEG C are warming up to 2 DEG C/min, and is incubated 2 hours, most
After cool to room temperature with the furnace, produce high-compactness Al-Doped ZnO target.
The observation (as shown in Figure 1) of electron scanning Electronic Speculum shows that prepared AZO powders are spherical, good dispersion, average
Particle diameter is~100nm.
The relative density of AZO targets made from the present embodiment is 99.6%, and resistivity is 7.2 × 10-4Ω cm, average crystalline substance
Size is 3~5 μm (typical microstructure figure is as shown in Figure 2).
Embodiment 2
The present embodiment provides a kind of preparation method of high densification Al-Doped ZnO target, 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) 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
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 100 DEG C, is incubated 50min, then 750 DEG C are warming up to 3 DEG C/min,
Insulation 3 hours, it is compressing after mist projection granulating, obtain biscuit；Compressing condition is：Pressure 125MPa, dwell time
8min；
(7) biscuit is sintered, the sintering condition is：1300 DEG C are warming up to 2 DEG C/min, and is incubated 3 hours, most
After cool to room temperature with the furnace, produce high-compactness Al-Doped ZnO target.
Electron scanning electron microscopic observation shows that prepared AZO powders are spherical, good dispersion, average grain diameter for~
115nm。
The relative density of AZO targets made from the present embodiment is 99.5%, and resistivity is 7.6 × 10-4Ω cm, average crystalline substance
Size is 4~6 μm.
Embodiment 3
The present embodiment provides a kind of preparation method of high densification Al-Doped ZnO target, 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) 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
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 200 DEG C, is incubated 30min, then 600 DEG C are warming up to 3 DEG C/min,
Insulation 5 hours, it is compressing after mist projection granulating, obtain biscuit；Compressing condition is：Pressure 200MPa, dwell time
15min；
(7) biscuit is sintered, the sintering condition is：1350 DEG C are warming up to 2 DEG C/min, and is incubated 1 hour, most
After cool to room temperature with the furnace, produce high-compactness Al-Doped ZnO target.
Electron scanning electron microscopic observation shows that prepared AZO powders are spherical, good dispersion, average grain diameter for~
85nm。
The relative density of AZO targets made from the present embodiment is 99.2%, and resistivity is 8.0 × 10-4Ω cm, average crystalline substance
Size is 5~7 μm.
Embodiment 4
The present embodiment provides a kind of preparation method of high densification Al-Doped ZnO target, comprises the following steps：
(1) compound concentration is 16g/L surface modification agent solution, is added in surface modification agent 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 coating material and Zn (NO3)2·6H2O weight ratio is
1：18；The coating material is that weight ratio is 1：2：1 soluble starch, polyethylene glycol and dodecyl sodium sulfate；
(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
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 160 DEG C, is incubated 35min, then 800 DEG C are warming up to 3 DEG C/min,
Insulation 3.5 hours, it is compressing after mist projection granulating, obtain biscuit；Compressing condition is：Pressure 175MPa, dwell time
10min；
(7) biscuit is sintered, the sintering condition is：1400 DEG C are warming up to 2 DEG C/min, and is incubated 2.5 hours,
Finally cool to room temperature with the furnace, produce high-compactness Al-Doped ZnO target.
Electron scanning electron microscopic observation shows that prepared AZO powders are spherical, good dispersion, average grain diameter for~
125nm。
The relative density of AZO targets made from the present embodiment is 99.8%, and resistivity is 7.0 × 10-4Ω cm, average crystalline substance
Size is 7~10 μm.
Embodiment 5
The present embodiment provides a kind of preparation method of high densification Al-Doped ZnO target, comprises the following steps：
(1) compound concentration is 18g/L surface modification agent solution, is added in surface modification agent 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 coating material and Zn (NO3)2·6H2O weight ratio is
1：19；The coating material is that weight ratio is 1：3 polyethylene glycol and dodecyl sodium sulfate；
(2) 92 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 180 DEG C, is incubated 35min, then 730 DEG C are warming up to 3 DEG C/min,
Insulation 4 hours, it is compressing after mist projection granulating, obtain biscuit；Compressing condition is：Pressure 130MPa, dwell time
13min；
(7) biscuit is sintered, the sintering condition is：1280 DEG C are warming up to 2 DEG C/min, and is incubated 2.5 hours,
Finally cool to room temperature with the furnace, produce high-compactness Al-Doped ZnO target.
Electron scanning electron microscopic observation shows that prepared AZO powders are spherical, good dispersion, average grain diameter for~
105nm。
The relative density of AZO targets made from the present embodiment is 99.8%, and resistivity is 7.0 × 10-4Ω cm, average crystalline substance
Size is 4~6 μm.
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 (7)
1. a kind of preparation method of high densification Al-Doped ZnO target, 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, it is compressing after mist projection granulating, obtain biscuit；
(7) biscuit is sintered, the sintering condition is：1200~1400 DEG C are warming up to 2 DEG C/min and insulation 1~5 is small
When, finally cool to room temperature with the furnace, produce high-compactness Al-Doped ZnO target.
2. a kind of preparation method of high densification Al-Doped ZnO target according to claim 1, it is characterised in that：It is described
Al and the Zn atomic percent are 3~5%.
3. a kind of preparation method of high densification Al-Doped ZnO target according to claim 1, it is characterised in that：It is described
Dressing agent is any one or a few in soluble starch, polyethylene glycol and dodecyl sodium sulfate.
4. a kind of preparation method of high densification Al-Doped ZnO target according to claim 3, it is characterised in that：It is described
The addition of dressing agent and Zn (NO3)2·6H2O weight ratio is 1：15~20.
5. a kind of preparation method of high densification Al-Doped ZnO target according to claim 1, it is characterised in that：It is described
The frequency range of ultrasonically treated ultrasonic wave is 40~60MHz in step (3).
6. a kind of preparation method of high densification Al-Doped ZnO target according to claim 1, it is characterised in that：It is described
Organic solvent in step (4) is that volume ratio is 1：3：5 ethanol, ethyl acetate and cyclohexanol.
7. a kind of preparation method of high densification Al-Doped ZnO target according to claim 1, it is characterised in that：It is described
The compressing condition of step (6) is：Pressure 100MPa~200MPa, dwell time 8min~15min.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112218840A (en) * | 2018-06-06 | 2021-01-12 | 杰富意矿物股份有限公司 | Zinc oxide powder for use in zinc oxide sintered body, and processes for producing these |
| CN110436915A (en) * | 2019-08-05 | 2019-11-12 | 北京航大微纳科技有限公司 | A kind of FBAR piezoelectric layer Zinc oxide doped target material and preparation method thereof |
| CN113402261A (en) * | 2021-06-04 | 2021-09-17 | 长沙壹纳光电材料有限公司 | IZO target precursor and preparation method and application thereof |
| CN113402261B (en) * | 2021-06-04 | 2022-06-21 | 长沙壹纳光电材料有限公司 | IZO target precursor and preparation method and application thereof |
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