CN102603285B - Preparation method of zinc oxide-based tubular rotary target material - Google Patents
Preparation method of zinc oxide-based tubular rotary target material Download PDFInfo
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- CN102603285B CN102603285B CN 201210041328 CN201210041328A CN102603285B CN 102603285 B CN102603285 B CN 102603285B CN 201210041328 CN201210041328 CN 201210041328 CN 201210041328 A CN201210041328 A CN 201210041328A CN 102603285 B CN102603285 B CN 102603285B
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Abstract
The invention relates to a preparation method of a zinc oxide-based tubular rotary target material. The preparation method comprises the following steps: taking NH4HCO3 as a precipitant, preparing pure zinc oxide powder and Al-doped zinc oxide powder with an atomic ratio of 1-7at% by a chemical precipitation method, presintering, conglomerating and shaping the powder, filling the powder into a mould, moulding the powder in a cold isostatic pressing manner at 300-340MPa, obtaining a biscuit with a relative density of 70-75%, sintering the biscuit under an oxidizing atmosphere, and processing the sintered biscuit to obtain the rotary target material. Compared with the prior art, the preparation method provided by the invention has the beneficial effects that the density of the biscuit is improved by 10-15%; the volume shrinkage in later stage sintering is reduced; the sintering deformation of the tubular target with a large length-diameter ratio is effectively controlled; and in the process of sintering, the circulating oxygen is served as a control atmosphere to avoid the component changing, large pores on the surface and density reduction caused by the large pores on the surface.
Description
Technical field
The present invention relates to a kind of preparation method of Zinc oxide-base tubulose rotary target material.
Background technology
ZnO is a kind of wide energy gap multifunctional semiconductor material, is considered to one of third generation semiconductor material.It has gas sensing property, pressure-sensitive, piezoelectricity, transparent conductivity, photo and is easy to multiple semiconductor material realizes excellent character such as integrated.The zno-based film of high-quality has characteristics such as band gap is wide, specific inductivity is low, temperature stability is good, light transmission rate is high, stable chemical performance, its abundant raw material is easy to get, nontoxic, cheap for manufacturing cost, it is mainly used: flat-panel display device, as LCD, OLED, contact panel etc.; Thin-film solar cells; Low-E (low radiation) energy saving building glass; The electromagnetic protection screen; Also obtained to use widely in other sides such as gas sensor, infrared stealth material, ultraviolet detectors in addition.
Compared to planar targets, 360 ° of target surfaces of rotary target material can be by even etching, and utilization ratio does not have sedimentary province again up to 80%, and coating quality and plated film temporal correlation are low, can accomplish higher sputter rate.The utilization ratio of planar targets only is 20%～30%.Along with the filming equipment technical progress, low-cost large-area, the Large-power High-Speed sputter prepares optoelectronic film becomes developing direction, and what match with it is to large size specification, high-quality sputtering target material demand.At present, be applied to thin-film solar cells and Low-E glass (low emissivity glass) Zinc oxide-base rotary target material commerical prod length and reached 3m so that longer, relative density will reach more than 98% at least.For ceramic rotary target material, be to be spliced by more piece, for given length, its required single-unit quantity is more few more good, and the splicing slit is more many, easily produces paradoxical discharge etc. in the high-speed high-power sputter, causes efficient to reduce the coating quality deterioration.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of Zinc oxide-base tubulose rotary target material, can prepare length-to-diameter ratio greater than 3, the zinc oxide-based ceramic rotary target material of target relative density 〉=99%, it is tiny that the target of preparation has homogeneous microstructure crystal grain, high heat shock resistance characteristics, can realize that Large-power High-Speed stablizes magnetron sputtering plating, thereby be applicable to the production of big area TCO plated film.
A kind of preparation method of Zinc oxide-base tubulose rotary target material, its special feature is, comprises the steps: with NH
4HCO
3Be precipitation agent, adopt chemical precipitation method to prepare pure zinc oxide powder and the Al doping zinc-oxide powder that contains the 1-7at% atomic ratio, pack into after the powder pre-burning conglomeration shaping in the mould, carry out cold isostatic compaction with 300-340MPa, make 70-75% relative density biscuit; Again biscuit behind the sintering, is namely got rotary target material through processing again in oxidizing atmosphere.
Wherein the zinc salt that uses in the chemical coprecipitation reaction is zinc sulfate or zinc nitrate.
Zn during wherein chemical coprecipitation reacts
2+Concentration is 1.5-2.0mol/L.
The Al doping zinc-oxide powder median size of the pure zinc oxide powder of wherein chemical precipitation prepared in reaction and 1-7at% is 100-200nm.
Wherein said pre-burning conglomeration shaping is at 850-1200 ℃ of following sintering 1-6hr, the shaping size-grade distribution between the 30-50 order, loose density 1.6-2.0g/cm
3
The assembling die be made up of steel inner core, jacket and ring plug of mould wherein, the material of jacket and ring plug is selected from any one in urethane, chloroprene rubber, nitrile rubber, PVC, organosilicon and the polyurethane.
Wherein oxidizing atmosphere is O
2Circulation atmosphere, wherein O
2Flow 30-300L/min.、
Wherein sintering condition is room temperature RT-850 ℃, and temperature rise rate 5-15 ℃/min, 850-1250 ℃, temperature rise rate 0.2-1 ℃/min, 1150-1450 ℃ of heat preservation sintering 20-30hr is cooled to 800 ℃ by rate of temperature fall 0.5-1 ℃/min afterwards then, afterwards cooling naturally.
Compared with prior art, preparation method of the present invention has following beneficial effect:
1, carries out the secondary microwave quick burning by 850-1200 ℃, form the presintering powder.This powder possesses in the sintering theory, the initial stage of sintering neck stage of growth, produced bigger volumetric shrinkage, particle closely contacts, grain diameter is not grown up as yet simultaneously, still keeps higher sintering activity, and biscuit density improves 10-15%, reduced volumetric shrinkage in the later stage sintering, the sintering warpage of big L/D ratio pipe target is effectively controlled;
2, in the calcining system, as controlled atmosphere, inhibited oxidation zinc volatilizees with circulation oxygen.Avoided composition to change and surperficial huge pore and the reduction of consequent density.Adopt room temperature-850 ℃, temperature rise rate 5-15 ℃/min, 850-1250 ℃, temperature rise rate 0.2-1 ℃/min, 1250-1450 ℃ of heat preservation sintering 20-30hr, lowers the temperature afterwards naturally by rate of temperature fall 0.5-1 ℃/min to 800 ℃.Guarantee that target changes fully mutually, eliminate internal stress, guarantee that geometrical shape is good and obtain the high-compactness sintered compact.
Description of drawings
Fig. 1 is presintering powder SEM figure among the embodiment 1;
Fig. 2 is assembling die synoptic diagram used among the embodiment 1.
Embodiment
Preparation method of the present invention finishes as follows:
1, zinc solution preparation: take by weighing quantitative metallic zinc (〉=4N) complete and be diluted to [Zn with deionized water with the pure 1+1 nitric acid dissolve of top grade
2+] concentration is 1.5-2.0mol/L;
2, aluminum salt solution preparation: according to Zn: Al=93-99: 1-7 (at%, atomic ratio) ratio, take by weighing Al (NO
3)
39H
2O (top grade is pure) is complete with anhydrous alcohol solution.If preparation pure zinc oxide powder, this step is omitted;
3, precipitant solution preparation: take by weighing quantitative NH
4HCO
3(top grade is pure), complete with deionized water dissolving, be mixed with 25% (wt/v%) solution;
4, change zinc solution and aluminum salt solution over to reactor, stir 20min, the conditioned reaction liquid temp is 30-45 ℃.
5, under the stirring velocity 300-600rpm/min, precipitant solution is added in zinc salt and the aluminium mixed salt solution with 10-20L/min speed, reaction 20-60min obtains reaction product;
6, reaction product is changed over to ceramic membrane washing and filtering machine, with the deionized water repetitive scrubbing, until washing supernatant liquor specific conductivity≤20 μ s, stop washing.The gained throw out is carried out spraying drying, obtain Al doping zinc-oxide precursor powder or pure zinc oxide precursor powder;
7, with precursor powder in 550 ℃ of microwave calcination 1hr, make oxide powder.Zirconia ball is situated between for mill, and dry ball milling 3-10hr carries out secondary microwave calcining 20min, formation presintering powder in 850-1000 ℃.Screen mill makes the interval groupization grain forming of 30-50 order powder, and loose density is controlled at 1.6-2.0g/cm
3
8, forming of green body: the powder mould of packing into, isostatic cool pressing pressure: 300-340MPa, pressurize 10min.Acquisition has the biscuit of 70-75% relative density; The assembling die that mould is made up of steel inner core 1, jacket 2 and ring plug 3,
9, with molding biscuit in O
2In the circulation atmosphere, 1250-1450 ℃ of sintering 20-30hr, wherein O
2Flow 30-200L/min;
10, by above-mentioned steps, obtain having high-compactness (relative density 〉=99%), length-to-diameter ratio＞3, high purity (99.99%), homogeneous microstructure, grain-size 5-10 μ m, phase structure zinc oxide-based sputtering target material.
Embodiment 1:
Take by weighing: metallic zinc 9830g (〉=4N) use the pure 1+1 of top grade (v/v%) nitric acid dissolve complete, and be diluted to [Zn with deionized water
2+] concentration is 1.2mol/L, is mixed with zinc solution; Take by weighing Al (NO
3)
39H
2O (top grade is pure) 2347g, adding 10L anhydrous alcohol solution is complete, is mixed with aluminum salt solution; Precipitant solution: take by weighing NH
4HCO
3(top grade is pure) 40000g is mixed with 25% (wt/v%) solution with deionized water.
Zinc solution and aluminum salt solution change reactor over to, stir 20min, and the conditioned reaction liquid temp is 35 ℃.Under the 400rpm mixing speed, precipitant solution is added in zinc salt and the aluminium mixed salt solution with 10L/min speed, being adjusted to ph value of reaction is 7.0-7.8, and reaction 60min obtains reaction product.Change reaction product over to ceramic membrane washing and filtering machine, with the deionized water repetitive scrubbing, until washing supernatant liquor specific conductivity≤20 μ s, stop washing.The gained throw out is carried out spraying drying, obtain Al doping zinc-oxide precursor powder.
With precursor powder in 550 ℃ of microwave calcination 1hr, make have the 100-150nm particle diameter, sphere or subsphaeroidal Al doping zinc-oxide powder.Be that mill is situated between with the zirconia ball, with above-mentioned powder dry ball milling 5hr, carry out secondary microwave calcining 20min in 1050 ℃, form the presintering powder.The pattern characteristic is seen accompanying drawing 2.Make the interval groupization grain forming of 30-50 order powder through screen mill, loose density is controlled at 1.6-2.0g/cm
3The powder mould of packing into, isostatic cool pressing pressure: 340MPa, pressurize 10min.Acquisition has the biscuit of 73% relative density.With molding biscuit in O
2In the circulation atmosphere, adopt room temperature (RT)-850 ℃, 10 ℃/min of temperature rise rate, 850-1250 ℃, 0.3 ℃/min of temperature rise rate, 1380 ℃ of heat preservation sintering 20hr, lower the temperature afterwards naturally by 1 ℃ of rate of temperature fall/min to 800 ℃.
Adopt Archimedes's method to measure density (theoretical density 5.61g/cm
3), relative density is 99.2%, the sintered compact specification: internal diameter 128mm, and height 420mm, wall thickness 18mm, the two ends id tolerance is less than 1%.
Embodiment 2:
Take by weighing: metallic zinc 10000g (〉=4N) use the pure 1+1 of top grade (v/v%) nitric acid dissolve complete, and be diluted to [Zn with deionized water
2+] concentration is 1.2mol/L, is mixed with zinc solution; Precipitant solution: take by weighing NH
4HCO
3(top grade is pure) 40000g is mixed with 25% (wt/v%) solution with deionized water.
Zinc solution and aluminum salt solution change reactor over to, stir 20min, and the conditioned reaction liquid temp is 40 ℃.Under the 400rpm mixing speed, precipitant solution is added in zinc salt and the aluminium mixed salt solution with 5L/min speed, being adjusted to ph value of reaction is 6.5-7.0, and reaction 60min obtains reaction product.Change reaction product over to ceramic membrane washing and filtering machine, with the deionized water repetitive scrubbing, until washing supernatant liquor specific conductivity≤20 μ s, stop washing.The gained throw out is carried out spraying drying, obtain the zinc oxide precursor powder.
With precursor powder in 600 ℃ of microwave calcination 1hr, make have the 150-200nm particle diameter, sphere or subsphaeroidal Zinc oxide powder.Be that mill is situated between with the zirconia ball, with above-mentioned powder dry ball milling 5hr, carry out secondary microwave calcining 40min in 900 ℃, form the presintering powder.Make the interval groupization grain forming of 30-50 order powder through screen mill, loose density is controlled at 1.6-2.0g/cm
3The powder mould of packing into, isostatic cool pressing pressure: 340MPa, pressurize 10min.Acquisition has the biscuit of 75% relative density.Isostatic cool pressing pressure: 340MPa, pressurize 10min.Acquisition has the biscuit of 75% relative density.With molding biscuit in O
2In the circulation atmosphere, adopt room temperature-850 ℃, 10 ℃/min of temperature rise rate, 850-1200 ℃, 0.2 ℃/min of temperature rise rate, 1200 ℃ of heat preservation sintering 10hr, lower the temperature afterwards naturally by 1 ℃ of rate of temperature fall/min to 800 ℃.
Adopt Archimedes's method to measure density (theoretical density 5.61g/cm
3), relative density is 99.4%, the sintered compact specification: internal diameter 128mm, and height 450mm, wall thickness 16mm, the two ends id tolerance is less than 1%.
Comparative example 1:
Integrated artistic flow process parameter is identical with embodiment 1, changes point and is precursor powder in 550 ℃ of microwave calcination 1hr, makes oxide powder.Direct cold isostatic compaction.The result is: biscuit density 60%; The sintering relative density is 98.3%, the sintered compact specification: internal diameter 128mm, and height 430mm, wall thickness 18mm, the two ends id tolerance is greater than 5%.
Claims (5)
1. the preparation method of a Zinc oxide-base tubulose rotary target material is characterized in that, comprises the steps: with NH
4HCO
3Be precipitation agent, adopt chemical precipitation method to prepare pure zinc oxide powder and the Al doping zinc-oxide powder that contains the 1-7at% atomic ratio, pack into after the powder pre-burning conglomeration shaping in the mould, carry out cold isostatic compaction with 300-340MPa, make 70-75% relative density biscuit, wherein said pre-burning conglomeration shaping is at 850-1200 ℃ of following sintering 1-6hr, the shaping size-grade distribution between the 30-50 order, loose density 1.6-2.0g/cm
3
Again biscuit behind the sintering, is namely got rotary target material through processing again in oxidizing atmosphere, wherein oxidizing atmosphere is O
2Circulation atmosphere, wherein O
2Flow 30-300L/min, and wherein sintering condition is room temperature RT-850 ℃, temperature rise rate 5-15 ℃/min, 850-1250 ℃, temperature rise rate 0.2-1 ℃/min, 1150-1450 ℃ of heat preservation sintering 20-30hr then, be cooled to 800 ℃ by rate of temperature fall 0.5-1 ℃/min afterwards, afterwards cooling naturally.
2. the preparation method of a kind of Zinc oxide-base tubulose rotary target material as claimed in claim 1, it is characterized in that: wherein the zinc salt that uses in the chemical precipitation method is zinc sulfate or zinc nitrate.
3. the preparation method of a kind of Zinc oxide-base tubulose rotary target material as claimed in claim 1 is characterized in that: Zn in the chemical precipitation method wherein
2+Concentration is 1.5-2.0 mol/L.
4. the preparation method of a kind of Zinc oxide-base tubulose rotary target material as claimed in claim 1 is characterized in that: wherein the pure zinc oxide powder of chemical precipitation method preparation and the Al doping zinc-oxide powder median size of 1-7at% are 100-200 nm.
5. the preparation method of a kind of Zinc oxide-base tubulose rotary target material as claimed in claim 1, it is characterized in that: the assembling die be made up of steel inner core (1), jacket (2) and ring plug (3) of mould wherein, the material of jacket (2) and ring plug (3) is selected from any one in urethane, chloroprene rubber, nitrile rubber, PVC, organosilicon and the polyurethane.
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| CN104987060B (en) * | 2015-06-18 | 2017-06-23 | 桂林电子科技大学 | Zinc oxide with back bone network structure is deposited with the preparation method of target |
| CN106676487B (en) * | 2016-10-09 | 2019-03-08 | 宁波森利电子材料有限公司 | A kind of zinc oxide-based ceramic sputtering target material and its preparation method and application |
| CN108151531B (en) * | 2017-09-11 | 2019-05-17 | 福建阿石创新材料股份有限公司 | A kind of the high temperature centrifugal sintering system and its sintering method of tubulose ITO target |
| CN108409340A (en) * | 2018-05-16 | 2018-08-17 | 郑州大学 | A kind of interior rotation high temperature sintering methods of tubular target |
| CN108530087A (en) * | 2018-05-16 | 2018-09-14 | 郑州大学 | A kind of Microwave Hybrid Heating of tubular target is interior to rotate high temperature sintering methods |
| JP7169776B2 (en) * | 2018-06-06 | 2022-11-11 | Koa株式会社 | Zinc oxide varistor and manufacturing method thereof |
| BE1027472B1 (en) * | 2019-07-31 | 2021-03-03 | Soc Ind Liegeoise Des Oxydes Sa | Process for preparing microspherules of an oxygenated zinc compound |
| CN114394818B (en) * | 2022-02-10 | 2022-10-18 | 江苏东玖光电科技有限公司 | Preparation method and manufacturing die of ITO (indium tin oxide) tubular target with large length-diameter ratio |
| CN114606470A (en) * | 2022-03-09 | 2022-06-10 | 涿州钢研昊普科技有限公司 | Lithium phosphate tube target and preparation method for integral forming of lithium phosphate tube target |
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| CN101705467A (en) * | 2009-05-14 | 2010-05-12 | 上海高展金属材料有限公司 | Method for preparing rotary ceramic target |
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| CN102276250A (en) * | 2010-05-21 | 2011-12-14 | 尤米科尔公司 | Aluminum doped zinc oxide sputtering targets |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101630553B (en) * | 2009-07-17 | 2011-10-12 | 立昌先进科技股份有限公司 | Preparation method of zinc oxide varister |
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|---|---|---|---|---|
| CN1370743A (en) * | 2001-10-30 | 2002-09-25 | 李国栋 | Production process of nano zinc oxide powder without coacervation |
| CN101705467A (en) * | 2009-05-14 | 2010-05-12 | 上海高展金属材料有限公司 | Method for preparing rotary ceramic target |
| CN102276250A (en) * | 2010-05-21 | 2011-12-14 | 尤米科尔公司 | Aluminum doped zinc oxide sputtering targets |
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