CN102312202B - A kind of Zinc oxide-based wide bandgap ceramic target and preparation method thereof - Google Patents
A kind of Zinc oxide-based wide bandgap ceramic target and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of Zinc oxide-based wide bandgap ceramic target and preparation method thereof, it is characterized in that adopting liquid phase method co-precipitation to prepare the ZnO nano powder of high sintering activity, utilize this nano-powder carrying out ultrahigh relative density sintering by unique sintering process lower than 900 DEG C for raw material, obtain rich Zn (or the scarce O of high-compactness
2) ZnO target.Based on this rich Zn (or scarce O
2) ZnO target, magnetically controlled DC sputtering can be utilized to instead of traditional rf magnetron sputtering and to prepare high resistant zno-based transparent film, can be widely used in transparent electron and Novel Optoelectronic Device field especially thin-film solar cells diffusion impervious layer and Window layer.The high-performance zinc oxide base ceramic target preparation technology that the present invention obtains is simple, with low cost, have very high transmitance and suitable resistivity, the target can prepared as high-performance high resistant zno-based transparent film, is with a wide range of applications at solar cell and field of photoelectric devices.
Description
Technical field
The present invention relates to a kind of Zinc oxide-based wide bandgap ceramic target and preparation method thereof, belong to broad stopband conducting semiconductor material preparation field.
Background technology
High resistance transparent ZnO film has a wide range of applications in transparent electron and Novel Optoelectronic Device field, in thin-film solar cells and photoelectric device, resistance within the specific limits ZnO film that is controlled, high permeability can be used as Window layer and diffusion impervious layer, can improve homogeneity and the stability of hull cell especially significantly.The method preparing high resistance transparent ZnO film at present has a lot: [(1) Y.J.Kim such as magnetron sputtering, pulsed light deposition (PLD), atomic layer epitaxy (ALE), gas phase epitaxy of metal organic compound (MOCVD), molecular beam epitaxy (MBE), C.H.Lee, et al.Appl.Phys.Lett.89 (2006) 163128; (2) X.N.Li, A.E.Sally, et al.J.Vac.Sci.Technol.A 24 (2006) 1213; (3) S.W.Kim, S.Z.Fujita, et al.Appl.Phys.Lett.88 (2006) 253114], wherein sputtering sedimentation is making ZnO film one of utilisation technology the most widely.
For sputtering method, the critical materials ZnO ceramic target preparing film accounts for very large production cost.At preparation of target materials and process aspect, hot isostatic pressing (HIP), the thermal pressed sintering molding process of the costliness that the early stage many employings of zno-based target are traditional, the normal pressure-sintered mode of the oriented low cost of recent technique obtains the development trend of the zno-based stupalith target of high-compactness, and usual sintering temperature is higher than 1300 degrees Celsius.In addition, the nano-powder preparation that sintering activity is high is one of key ensureing high-performance transparent conductive film, in the preparation of target, as mentioned above, the normal pressure-sintered mode of low cost obtains the development trend of the zno-based stupalith target of high-compactness, and high-compactness reduces the generation of " stain " (Nodules) in deposition process, improves the key of yield rate and film quality.
In traditional technique, general employing intrinsic ZnO ceramic target, because intrinsic ZnO is wide bandgap semiconductor (3.3eV), commercial ceramic target resistance is very high and substantially close to state of insulation, thus traditional preparation methods all adopts radio-frequency magnetron sputter method [(4) J.Ch.Lee, K.H.Kang, etc.Solar EnergyMaterials & Solar Cells 64 (2000) 185].And for the application of industry member, radio-frequency power supply is due to expensive and be difficult to be used on a large scale.Comparatively speaking; in large-scale industrial is produced; direct supply platform has higher process consistency and controlling functions; single with regard to CIGS (copper indium gallium tin) thin-film solar cells window layer material; if high resistant ZnO (i-ZnO) and low-resistance window electrode are as adopted magnetically controlled DC sputtering; then not only can reduce costs, also can greatly reduce technique change, and then improve output.
Based on the existing Problems existing of above-described intrinsic zno-based stupalith target and development trend, the anxious rich Zn or scarce O in a kind of broad stopband to be developed
2zrO ceramic target, can design of the present invention be when preparing high resistant zno-based transparent film, adopt direct current magnetron sputtering process to carry out depositing and not needing expensive radio-frequency magnetron sputter method.For this reason, the present inventor intends the technology developing the nano-powders such as liquid phase method controlled synthesis ZnO.By optimizing the influence conditions such as reactant concn, drying conditions, anneal temperature and time, achieving and there is controlled grain size (particle diameter 20 ~ 200nm), single crystal phase structure, homodisperse zno-based nano-powder preparation technology.On this basis, by special compacting, sintering process, under lower than 900 DEG C of conditions sintering obtain density higher than 95% rich Zn (or scarce O
2) Zinc oxide-based wide bandgap ceramic target.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of zinc-oxide-base wide-bandgap stupalith target and preparation method thereof is provided.The design of invention is: adopt liquid phase method co-precipitation to prepare the ZnO nano powder of high sintering activity, utilizes this nano-powder carrying out ultrahigh relative density sintering by unique sintering process lower than 900 DEG C for raw material, obtains rich Zn (or the scarce O of high-compactness
2) ZnO target.Namely its structure is Zn
1+xo or ZnO
1-x, 0.05 < X≤0.2.This broad stopband ceramic target is rich Zn (or scarce O
2) structure, prepared ZnO ceramic target resistivity is 10
-1-10
3dEG C cm can utilize magnetically controlled DC sputtering to replace traditional rf magnetron sputtering to prepare high resistant zno-based transparent film.
The present invention is described below in detail.
A) material preparation
Rich Zn prepared by the present invention (or scarce O
2) ZnO target, the magnetron sputtering method comprising magnetically controlled DC sputtering can be adopted to prepare N-shaped high resistant zno-based transparent film, be applied to transparent electron and Novel Optoelectronic Device field.Concrete steps are as follows:
1., ZnO forerunner's nano-powder of Liquid preparation methods high sintering activity
A) prepared burden according to mol ratio in zinc source and oxygen source, utilize soft chemical solution method, hydrothermal method or sol-gel method, and carry out coprecipitation reaction;
Described zinc source is one or more in metallic zinc, zinc oxide, zinc acetate, zinc oxalate, zinc citrate, zinc nitrate, zinc sulfate, zinc fluoride and zinc chloride etc.;
Described oxygen source is medium one or more of ammoniacal liquor, sodium hydroxide, potassium hydroxide, urea, thiocarbamide and hydrazine;
B) the nano-ZnO precursor powder of high reactivity, high crystalline is obtained further across mixing, oven dry and grinding; And the presoma powder grain size of preparation is 20-200nm, and grain dispersion is even.
2., the rich Zn of high-performance (or scarce O
2) ZnO ceramic target technology of preparing
A) by high performance precursor powder granulation, by means moulded sections such as isostatic pressed, the biscuit of ceramics of high compacted density is prepared;
B) adopting upper and lower two crucibles, in lower crucible, sink to graphite, being inverted in inserting the ZnO biscuit of ceramics suppressed in upper crucible on lower crucible.Adopt and sinter less than or equal under the sintering temperature of 900 DEG C, be specially the sintering temperature of 500 ~ 900 DEG C, in sintering process, be anaerobic environment in the enclosed space that upper and lower two crucibles are formed, graphite easily forms the CO gas of reductibility simultaneously, thus causes target in preparation process, form anoxic or rich Zn state.
C) sintering temperature, time and atmosphere is regulated, after the sintering of 2 ~ 24 hours, i.e. rich Zn (or the scarce O of obtained high compactness
2) zinc-oxide-base wide-bandgap stupalith target.
B) sample characterization and performance evaluation
1., morphology characterization
Pass through scanning electron microscopic observation its surface or cross-section morphology to gained nano-powder of the present invention and ceramic target sample, Electronic Speculum model used is LEO-1530VP.
2., electric property characterizes
Gained target material of the present invention is sampled and after putting silver electrode, utilizes Hall effect to adopt vanderburg four probe method (Accent HL5500 Hall instrument) to carry out conductivity evaluation.
Accompanying drawing explanation
Fig. 1 schemes according to ZnO forerunner's nano powder surface pattern SEM of high sintering activity provided by the invention;
Fig. 2 according to density provided by the invention higher than 95% zno-based nano ceramics target Cross Section Morphology SEM scheme.
Embodiment
Introduce embodiments of the invention below, to increase further understanding of the present invention, but the present invention is limited to embodiment absolutely not.Every technical scheme belonging to content of the present invention and be equal to, all belongs to the protection domain of this patent.
Embodiment 1:
Zinc source and oxygen source are prepared burden according to mol ratio and carries out coprecipitation reaction, the nano-ZnO precursor powder of high reactivity, high crystalline is obtained again through mixing, oven dry and grinding, then by high performance precursor powder granulation, by means moulded sections such as isostatic pressed, prepare the biscuit of ceramics of high compacted density.Adopting upper and lower two crucibles, in lower crucible, sink to graphite, being inverted in inserting the ZnO biscuit of ceramics suppressed in upper crucible on lower crucible.Adopt the sintering temperature of 750 DEG C, in sintering process, be anaerobic environment in the enclosed space that upper and lower two crucibles are formed, graphite easily forms the CO gas of reductibility simultaneously, thus causes target in preparation process, form anoxic or rich Zn state.After the sintering of 16 hours, i.e. obtained anoxic state ZnO
0.9the broad stopband stupalith target of structure.
Fig. 1 is that ZnO forerunner's nano powder surface pattern SEM of high sintering activity schemes, and can see, ZnO precursor powder grain-size prepared by the present invention is that between particle diameter 20 ~ 50nm, grain dispersion is even.Fig. 2 is that zno-based ceramic target Cross Section Morphology SEM schemes, and graphical results shows, and nano ceramics target density is higher than 95%.The test result of electrical property shows, under this implementation condition, obtained ceramic target resistivity about 120 Ω cm, meets the magnetic control spattering target application requiring comprising magnetically controlled DC sputtering.
Embodiment 2:
Zinc source and oxygen source are prepared burden according to mol ratio and carries out coprecipitation reaction, the nano-ZnO precursor powder of high reactivity, high crystalline is obtained again through mixing, oven dry and grinding, then by high performance precursor powder granulation, by means moulded sections such as isostatic pressed, prepare the biscuit of ceramics of high compacted density.Adopting upper and lower two crucibles, in lower crucible, sink to graphite, being inverted in inserting the ZnO biscuit of ceramics suppressed in upper crucible on lower crucible.Adopt the sintering temperature of 900 DEG C, in sintering process, be anaerobic environment in the enclosed space that upper and lower two crucibles are formed, graphite easily forms the CO gas of reductibility simultaneously, thus causes target in preparation process, form anoxic or rich Zn state.After the sintering of 2 hours, i.e. obtained anoxic state ZnO
0.88the broad stopband stupalith target of structure.ZnO precursor powder grain-size prepared by the present invention is between particle diameter 20 ~ 50nm, and nano ceramics target density is higher than 95%, suitable with embodiment 1.The test result of electrical property shows, under this implementation condition, obtained ceramic target resistivity about 95 Ω cm, slightly lower than embodiment 1, meets the magnetic control spattering target application requiring comprising magnetically controlled DC sputtering.
Embodiment 3:
Zinc source and oxygen source are prepared burden according to mol ratio and carries out coprecipitation reaction, the nano-ZnO precursor powder of high reactivity, high crystalline is obtained again through mixing, oven dry and grinding, then by high performance precursor powder granulation, by means moulded sections such as isostatic pressed, prepare the biscuit of ceramics of high compacted density.Adopting upper and lower two crucibles, in lower crucible, sink to graphite, being inverted in inserting the ZnO biscuit of ceramics suppressed in upper crucible on lower crucible.Adopt the sintering temperature of 850 DEG C, in sintering process, be anaerobic environment in the enclosed space that upper and lower two crucibles are formed, graphite easily forms the CO gas of reductibility simultaneously, thus causes target in preparation process, form anoxic or rich Zn state.After the sintering of 20 hours, i.e. obtained rich zinc state Zn
1.13the broad stopband stupalith target of O structure.ZnO precursor powder grain-size prepared by the present invention is between particle diameter 20 ~ 50nm, and nano ceramics target density is higher than 95%, suitable with embodiment 1.The test result of electrical property shows, under this implementation condition, obtained ceramic target resistivity about 9.6 Ω cm, lower than embodiment 1, meets the magnetic control spattering target application requiring comprising magnetically controlled DC sputtering.
Embodiment 4:
Zinc source and oxygen source are prepared burden according to mol ratio and carries out coprecipitation reaction, the nano-ZnO precursor powder of high reactivity, high crystalline is obtained again through mixing, oven dry and grinding, then by high performance precursor powder granulation, by means moulded sections such as isostatic pressed, prepare the biscuit of ceramics of high compacted density.Adopting upper and lower two crucibles, in lower crucible, sink to graphite, being inverted in inserting the ZnO biscuit of ceramics suppressed in upper crucible on lower crucible.Adopt the sintering temperature of 500 DEG C, in sintering process, be anaerobic environment in the enclosed space that upper and lower two crucibles are formed, graphite easily forms the CO gas of reductibility simultaneously, thus causes target in preparation process, form anoxic or rich Zn state.After the sintering of 24 hours, i.e. obtained anoxic state ZnO
0.92the broad stopband stupalith target of structure.ZnO precursor powder grain-size prepared by the present invention is between particle diameter 50 ~ 100nm, and a little more than embodiment 1, nano ceramics target density is higher than 95%.The test result of electrical property shows, under this implementation condition, obtained ceramic target resistivity about 520 Ω cm, higher than embodiment 1, meets the magnetic control spattering target application requiring comprising magnetically controlled DC sputtering.
Embodiment 5:
Zinc source and oxygen source are prepared burden according to mol ratio and carries out coprecipitation reaction, the nano-ZnO precursor powder of high reactivity, high crystalline is obtained again through mixing, oven dry and grinding, then by high performance precursor powder granulation, by means moulded sections such as isostatic pressed, prepare the biscuit of ceramics of high compacted density.Adopting upper and lower two crucibles, in lower crucible, sink to graphite, being inverted in inserting the ZnO biscuit of ceramics suppressed in upper crucible on lower crucible.Adopt the sintering temperature of 900 DEG C, in sintering process, be anaerobic environment in the enclosed space that upper and lower two crucibles are formed, graphite easily forms the CO gas of reductibility simultaneously, thus causes target in preparation process, form anoxic or rich Zn state.After the sintering of 24 hours, i.e. obtained rich zinc state Zn
1.2the broad stopband stupalith target of O structure.ZnO precursor powder grain-size prepared by the present invention is between particle diameter 20 ~ 40nm, and a little less than embodiment 1, nano ceramics target density is higher than 95%.The test result of electrical property shows, under this implementation condition, obtained ceramic target resistivity about 0.9 Ω cm, lower than embodiment 1, meets the magnetic control spattering target application requiring comprising magnetically controlled DC sputtering.
Embodiment 6:
Zinc source and oxygen source are prepared burden according to mol ratio and carries out coprecipitation reaction, the nano-ZnO precursor powder of high reactivity, high crystalline is obtained again through mixing, oven dry and grinding, then by high performance precursor powder granulation, by means moulded sections such as isostatic pressed, prepare the biscuit of ceramics of high compacted density.Adopting upper and lower two crucibles, in lower crucible, sink to graphite, being inverted in inserting the ZnO biscuit of ceramics suppressed in upper crucible on lower crucible.Adopt the sintering temperature of 650 DEG C, in sintering process, be anaerobic environment in the enclosed space that upper and lower two crucibles are formed, graphite easily forms the CO gas of reductibility simultaneously, thus causes target in preparation process, form anoxic or rich Zn state.After the sintering of 10 hours, i.e. obtained anoxic state ZnO
0.95the broad stopband stupalith target of structure.ZnO precursor powder grain-size prepared by the present invention is between particle diameter 50 ~ 200nm, and higher than embodiment 1, nano ceramics target density is higher than 95%.The test result of electrical property shows, obtained ceramic target resistivity about 1.05 × 10 under this implementation condition
3Ω cm, higher than embodiment 1, meets the magnetic control spattering target application requiring comprising magnetically controlled DC sputtering.
Embodiment 7:
Zinc source and oxygen source are prepared burden according to mol ratio and carries out coprecipitation reaction, the nano-ZnO precursor powder of high reactivity, high crystalline is obtained again through mixing, oven dry and grinding, then by high performance precursor powder granulation, by means moulded sections such as isostatic pressed, prepare the biscuit of ceramics of high compacted density.Adopting upper and lower two crucibles, in lower crucible, sink to graphite, being inverted in inserting the ZnO biscuit of ceramics suppressed in upper crucible on lower crucible.Adopt the sintering temperature of 900 DEG C, in sintering process, be anaerobic environment in the enclosed space that upper and lower two crucibles are formed, graphite easily forms the CO gas of reductibility simultaneously, thus causes target in preparation process, form anoxic or rich Zn state.After the sintering of 10 hours, i.e. obtained rich zinc state Zn
1.09the broad stopband stupalith target of O structure.ZnO precursor powder grain-size prepared by the present invention is between particle diameter 20 ~ 50nm, and nano ceramics target density is higher than 95%, suitable with embodiment 1.The test result of electrical property shows, under this implementation condition, obtained ceramic target resistivity about 82 Ω cm, lower than embodiment 1, meets the magnetic control spattering target application requiring comprising magnetically controlled DC sputtering.
Claims (5)
1. a Zinc oxide-based wide bandgap ceramic target preparation method, described ceramic target is the zinc oxide of rich zinc or anoxic, and structural formula is Zn
1+xo or ZnO
1-x, 0.05 < X≤0.2, has 10
-1-10
3the resistivity of Ω .cm, comprises the following steps:
A) prepared burden according to mol ratio in zinc source and oxygen source, then obtain the nano-ZnO precursor powder of high reactivity, high crystalline through mixing, oven dry and grinding;
B) step a prepare by high performance precursor powder granulation, by the moulded section of isostatic pressed means, prepare the biscuit of ceramics of high compacted density;
C) adopt upper and lower two crucibles, in lower crucible, sink to graphite, in upper crucible, insert ZnO biscuit of ceramics that step b suppresses and be inverted on lower crucible; Adopt and sinter less than or equal under the sintering temperature of 900 DEG C, obtained described rich Zn or anoxic zinc-oxide-base wide-bandgap stupalith target;
Described zinc source be selected from metallic zinc, zinc oxide, zinc acetate, zinc oxalate, zinc citrate, zinc nitrate, zinc sulfate, zinc fluoride and zinc chloride one or more;
Described oxygen source is: one or more in ammoniacal liquor, sodium hydroxide, potassium hydroxide, urea, thiocarbamide and hydrazine.
2., by the preparation method of target according to claim 1, it is characterized in that the sintering temperature that step c adopts is 500-900 DEG C.
3., by the preparation method of target according to claim 1, it is characterized in that sintering time is 2-24 hour under described sintering temperature.
4., by the preparation method of target according to claim 1, it is characterized in that the density > 95% of the zinc oxide target of rich zinc or the anoxic obtained.
5., by the preparation method of target according to claim 1, it is characterized in that the grain-size of ZnO precursor prepared by step a is 20-200nm.
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| CN103724008A (en) * | 2013-12-13 | 2014-04-16 | 西北稀有金属材料研究院 | Pure zinc oxide ceramic sputtering target material and preparation method thereof |
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