CN104451582B - A kind of electric conductive oxidation zirconium rotary target material and preparation method thereof - Google Patents
A kind of electric conductive oxidation zirconium rotary target material and preparation method thereof Download PDFInfo
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- CN104451582B CN104451582B CN201410841672.5A CN201410841672A CN104451582B CN 104451582 B CN104451582 B CN 104451582B CN 201410841672 A CN201410841672 A CN 201410841672A CN 104451582 B CN104451582 B CN 104451582B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- Coating By Spraying Or Casting (AREA)
Abstract
The invention provides a kind of electric conductive oxidation zirconium rotary target material, the target material composition is ZrOx, the target density is 5.18-5.8g/cm3, wherein, 1.2≤X≤1.8.Present invention also offers a kind of preparation method of electric conductive oxidation zirconium rotary target material, including：The preparation of zirconium oxide spray coating powder；Spray the processing of matrix；Spray prime coat；With plasma spray coating process zirconia coating is sprayed on spraying matrix.The electric conductive oxidation zirconium rotary target material that the present invention is provided, target material structure is fine and close, composition is uniform, good conductivity, flawless, and it sprays length and diameter is unrestricted, and thickness can reach 13mm, and density is 5.18-5.8g/cm3, and the preparation method of electric conductive oxidation zirconium rotary target material that the present invention is provided, production process is simple and convenient, and cost is relatively low.
Description
Technical field
The present invention relates to technical field of material, in particular to a kind of electric conductive oxidation zirconium rotary target material and its system
Preparation Method.
Background technology
Magnetron sputtering is generally divided into two kinds：D.c. sputtering and radio-frequency sputtering, wherein d.c. sputtering are merely able to sputter conduction material
Material, but its equipment principle is simple, and in splash-proofing sputtering metal, its speed is also fast；And the use scope of radio-frequency sputtering is more extensive, except can
Sputter conductive material outside, can also sputter non-conductive material, at the same can also carry out reactive sputtering prepare oxide, nitride and
The compound-materials such as carbide.Because metal targets need to use oxidation anti-when producing high refractive index film using sputtering method
Sull should could be generated, technics comparing is complicated and is difficult to the film of acquirement excellent properties, and ordinary oxide is one
As in the case of be insulating materials, radio-frequency sputtering technique can only be used by preparing high refractive index film using ordinary oxide target, difficult
To obtain higher sputter rate.
Rotary target material have the advantages that relative to planar targets it is a lot, 1) flat target utilization rate is low, can reach 35-
40%, flat target changes frequent, can increase process for large-scale production and be unfavorable for plant maintenance, influences production capacity.And rotate
Target utilization rate is high, can reach more than 70%, maintenance period is long, production capacity is high, it is to avoid the shortcoming of flat target；2) sputtering rate
It hurry up, be 2-3 times of flat target；3) arc is beaten in effective reduction and surface is scaling-off, and technology stability is good etc..
For rotary plating target, it is desirable to rotary target material be single entirety, or segmentation be welded on same bushing pipe.With current
Technical conditions, the preparation method of rotary target material mainly includes：Hot isostatic pressing method, hot pressing sintering method and casting method, process above are each
Have an advantage and disadvantage, but be difficult to meet for various sizes of flexible control, especially hot pressing sintering method can only production length be
Single branch target within 300mm, therefore certain length requirement can only be reached on bushing pipe by more piece segmentation Bonding,
The step of so adding production, improves the cost of target production.
Plasma spraying rotary target material, is that metal or nonmetallic spray coating powder are heated into fusing or half in plasma flame flow
Molten state, and in company with plasma flame flow, with spray at a high speed and deposit to it is pre- first pass through on treated workpiece surface, with past
Multiple lasting spraying, can obtain certain thickness target.Because plasma spraying temperature is high, all infusibilities can be almost sprayed
Metal and ceramic powders；And spraying process is one-shot forming, the size for spraying target is unrestricted, and step is simple, convenient spirit
It is living.
The content of the invention
The technical problems to be solved by the invention are to provide that a kind of production process is simple and convenient, lower-cost electric conductive oxidation
Zirconium rotary target material and preparation method thereof.
In order to solve the above technical problems, the invention provides a kind of electric conductive oxidation zirconium rotary target material, the target material composition is
ZrOx, the target density is 5.18-5.8g/cm3, wherein, 1.2≤X≤1.8.
Present invention also offers a kind of preparation method of electric conductive oxidation zirconium rotary target material, comprise the following steps：
The preparation of zirconium oxide spray coating powder；
Spray the processing of matrix；
Spray prime coat；
With plasma spray coating process zirconia coating is sprayed on spraying matrix.
Further, the preparation of the zirconium oxide spray coating powder includes：By percentage to the quality, by 93-98% zirconium oxide
After powder is mixed with 2-7% carbon dust, sintered 6-10 hours in 1500-1700 DEG C of hydrogen atmosphere, it is then spray-dried,
Obtain the zirconium oxide spray coating powder of 100-400 mesh.
Further, the purity of the Zirconium oxide powder is not less than 99.5wt%, and particle diameter is 1-5um.
Further, the processing of the spraying matrix includes：First clean, polishing removes the oil stain of the spraying matrix surface
And oxide layer, the spraying matrix surface is then roughened using sandblasting.
Further, the spraying prime coat is the alloy coat that 0.1-0.3mm is sprayed in spraying matrix surface.
Further, the spraying alloy coat is in the spraying matrix surface spraying nickel bag using plasma spraying method
Aluminium, nickel chromium triangle, nickel chromium triangle aluminium or nichrome-chromium-aluminium-yttrium powder, or closed using arc process in the spraying matrix surface spraying aluminium bronze or nickel aluminium
Spun gold.
Further, it is described during the use plasma spray coating process sprays zirconia coating on spraying matrix
The rotating speed control for spraying matrix is 30-80r/min, and the distance controlling between spray gun and the spraying matrix is 120-200mm, spray gun
Translational speed control be 300-800mm/min.
Further, it is described during the use plasma spray coating process sprays zirconia coating on spraying matrix
Spraying matrix surface is cooled down with compressed air stream, and the surface temperature control of the spraying matrix is no more than 200 DEG C.
A kind of electric conductive oxidation zirconium rotary target material that the present invention is provided, target material structure is fine and close, composition is uniform, good conductivity, nothing
Crackle, it sprays length and diameter is unrestricted, and thickness can reach 13mm, and density is 5.18-5.8g/cm3, and the present invention carries
The preparation method of the electric conductive oxidation zirconium rotary target material of confession, production process is simple and convenient, and cost is relatively low.
Brief description of the drawings
Fig. 1 is a kind of preparation flow figure of electric conductive oxidation zirconium rotary target material provided in an embodiment of the present invention.
Embodiment
A kind of electric conductive oxidation zirconium rotary target material provided in an embodiment of the present invention, the target material composition is ZrOx, the target is close
Spend for 5.18-5.8g/cm3, wherein, 1.2≤X≤1.8.
Referring to the preparation method of Fig. 1, the present invention a kind of electric conductive oxidation zirconium rotary target material provided, including following technique step
Suddenly：
The preparation of zirconium oxide spray coating powder：It is that to be not less than 99.95wt%, particle diameter be 1- for 93-98%, purity by mass percent
After the carbon dust mechanical mixture that 5um Zirconium oxide powder is 2-7% with mass percent, in 1500-1700 DEG C of hydrogen atmosphere
Sintering 6-10 hours, it is then spray-dried, obtain the dusty spray of 100-400 mesh.
Spray the processing of matrix：Being removed with cleaning and mechanical grinding method includes surface oil stain and oxide layer, then utilizes spray
Sand makes matrix surface reach certain roughness, to increase the bond strength of matrix and coating.
Spray prime coat：Plasma spraying method is used to spray nickel of a layer thickness for 0.1-0.5mm in spraying matrix surface
Alclad (Ni/Al), nickel chromium triangle (Ni/Cr), nickel chromium triangle aluminium (Ni/Cr/Al) or nichrome-chromium-aluminium-yttrium (Ni/Cr/Al/Y) alloy coat, or adopt
With arc spraying the aluminium bronze or ni-al alloyed wire that a layer thickness is 0.1-0.5mm are sprayed in spraying matrix surface.Wherein spray
Apply prime coat during, spraying matrix rotate around central shaft, spray gun with spraying matrix maintain a certain distance and along spray matrix
Back and forth at the uniform velocity moved back and forth with certain speed in direction.
With plasma spray coating process zirconia coating is sprayed on spraying matrix：Matrix is sprayed in spraying process with 30-
80r/min rotating speed is rotated around central shaft, and 120-200mm distance, and the spray of spray gun edge are kept between spray gun and spraying matrix
Matrix direction is applied back and forth at the uniform velocity to move back and forth with 300-800mm/min speed.Simultaneously in spraying matrix in spraying process
Surface is cooled down with compressed air, controls its surface temperature to be no more than 200 DEG C.With plasma spray coating process on spraying matrix
The design parameter for spraying zirconia coating is as shown in table 1.
The plasma spraying method of table 1 prepares zirconium oxide rotary target material parameter
Electric conductive oxidation zirconium rotary target material provided below by embodiment the present invention and preparation method thereof is illustrated.
Embodiment 1
It is 133mm in external diameter, length is the zirconium oxide target that coating thickness is 4mm on 3191mm stainless steel tube.
It is that 98wt%, purity are not less than the Zirconium oxide powder and quality hundred that 99.5wt%, particle diameter are 1um by mass percent
Divide than the carbon dust for 2wt% after mechanical mixture, hydrogen sintering 6h is led at 1500 DEG C, powder is through spraying after then sintering
Drying-granulating obtains the zirconium oxide spray coating powder of 100-225 mesh.
Surface oil stain is removed with absolute ethyl alcohol, sandblasting, matrix surface is reached certain roughness.
0.1mm nickel-chromium-aluminum-yttrium coatings are sprayed with plasma spraying method, parameter is as shown in table 2.
The plasma spraying nichrome-chromium-aluminium-yttrium bottoming layer parameter of table 2
Zirconium oxide spray coating powder is sprayed on the basal body pipe for being coated with prime coat with plasma spraying method, target material surface
Cooled down with compressed air, control target material surface temperature is at 180 DEG C.The spray parameters of zirconium oxide rotary target material are as shown in table 3.
The plasma spraying of table 3 prepares zirconium oxide rotary target material parameter
Zirconium oxide rotary target material prepared by this example is black, and compact structure, composition is uniform, flawless；Thickness 4.3mm；
It is 5.32g/cm with Archimedes's drainage detection density3, it is fully oxidized by being heated in oxygen atmosphere, survey weightening finish method and obtain
The composition of target is ZrO1.8。
Embodiment 2
It is 165mm in external diameter, length is the zirconium oxide target that coating thickness is 6mm on 2791mm stainless steel tube.
It is that 95wt%, purity are not less than the Zirconium oxide powder and quality hundred that 99.5wt%, particle diameter are 3um by mass percent
Divide than the carbon dust for 5wt% after mechanical mixture, hydrogen sintering 8h is led at 1600 DEG C, powder is through spraying after then sintering
Drying-granulating obtains the zirconium oxide spray coating powder of 140-325 mesh.
Surface oil stain is removed with absolute ethyl alcohol, sandblasting, matrix surface is reached certain roughness.
0.3mm nickel chromium triangle coatings are sprayed with plasma spraying method, parameter is as shown in table 4.
The plasma spraying nickel chromium triangle bottoming layer parameter of table 4
Zirconium oxide spray coating powder is sprayed on the basal body pipe for being coated with prime coat with plasma spraying method, target material surface
Cooled down with compressed air, control target material surface temperature is at 190 DEG C.The spray parameters of zirconium oxide rotary target material are as shown in table 5.
The plasma spraying of table 5 prepares zirconium oxide rotary target material parameter
Zirconium oxide rotary target material prepared by this example is black, and compact structure, composition is uniform, flawless；Thickness 6.1mm；
It is 5.02g/cm with Archimedes's drainage detection density3, it is fully oxidized by being heated in oxygen atmosphere, survey weightening finish method and obtain
The composition of target is ZrO1.6。
Embodiment 3
It is 173mm in external diameter, length is that coating thickness is the thick zirconium oxide targets of 10mm on 2550mm stainless steel tube.
It is that 94wt%, purity are not less than 99.5wt% by mass percent, particle diameter is to mix in 3um or so Zirconium oxide powder
Enter 6wt% carbon dust, lead to hydrogen sintering 8h at 1650 DEG C after mechanical mixture, powder is spray-dried after then sintering
Granulation obtains the zirconium oxide spray coating powder of 140-325 mesh.
Surface oil stain is removed with absolute ethyl alcohol, sandblasting, matrix surface is reached certain roughness.
0.4mm nickel aluminium coatings are sprayed with arc spraying, parameter is as shown in table 6.
The arc spraying of table 6 sprays the parameter of 0.4mm nickel aluminium coatings：
| Technological parameter | Electric current/A | Voltage/V | Silk material diameter | Wire feed rate | Supply gas pressure |
| Parameter value | 200 | 50 | 2.5mm | 100mm/s | 0.5MPa |
Zirconium oxide spray coating powder is sprayed on the basal body pipe for being coated with prime coat with plasma spraying method, target material surface
Cooled down with compressed air, control target material surface temperature is below 180 DEG C.The spray parameters of zirconium oxide rotary target material such as table 7
It is shown.
The plasma spraying of table 7 prepares zirconium oxide rotary target material parameter
Zirconium oxide rotary target material prepared by this example is black, and compact structure, composition is uniform, flawless；Thickness 9.8mm；
It is 5.27g/cm with Archimedes's drainage detection density3, it is fully oxidized by being heated in oxygen atmosphere, survey weightening finish method and obtain
The composition of target is ZrO1.3。
Embodiment 4
It is 133mm in external diameter, length is that coating thickness is the thick zirconium oxide targets of 13mm on 1550mm stainless steel tube.
It is that 93wt%, purity are not less than Zirconium oxide powder and the matter that 99.5wt%, particle diameter are 5um or so by mass percent
The carbon dust that amount percentage is 7wt% leads to hydrogen sintering 10h after mechanical mixture at 1700 DEG C, powder after then sintering
It is spray-dried to granulate the zirconium oxide spray coating powder for obtaining 240-400 mesh.
Surface oil stain is removed with absolute ethyl alcohol, sandblasting, matrix surface is reached certain roughness.
0.5mm nickel aluminium coatings are sprayed with arc spraying, parameter is as shown in table 8.
The parameter of the electric arc spraying ni-al alloyed wire prime coat of table 8：
| Technological parameter | Electric current/A | Voltage/V | Silk material diameter | Wire feed rate | Supply gas pressure |
| Parameter value | 200 | 50 | 3mm | 150mm/s | 0.6MPa |
Zirconium oxide spray coating powder is sprayed on the basal body pipe for being coated with prime coat with plasma spraying method, target material surface
Cooled down with compressed air, control target material surface temperature is at 195 DEG C.The spray parameters of zirconium oxide rotary target material are as shown in table 9.
The plasma spraying of table 9 prepares zirconium oxide rotary target material parameter
Zirconium oxide rotary target material prepared by this example is black, and compact structure, composition is uniform, flawless；Thickness 12.8mm；
It is 5.27g/cm with Archimedes's drainage detection density3, it is fully oxidized by being heated in oxygen atmosphere, survey weightening finish method and obtain
The composition of target is ZrO1.2。
It should be noted last that, above embodiment is merely illustrative of the technical solution of the present invention and unrestricted,
Although the present invention is described in detail with reference to example, it will be understood by those within the art that, can be to the present invention
Technical scheme modify or equivalent substitution, without departing from the spirit and scope of technical solution of the present invention, it all should cover
Among scope of the presently claimed invention.
Claims (6)
1. a kind of preparation method of electric conductive oxidation zirconium rotary target material, it is characterised in that comprise the following steps：
The preparation of zirconium oxide spray coating powder；
Spray the processing of matrix；
Spray prime coat；
With plasma spray coating process zirconia coating is sprayed on spraying matrix；
During the use plasma spray coating process sprays zirconia coating on spraying matrix, the rotating speed of the spraying matrix
Control as 30-80r/min, the distance controlling between spray gun and the spraying matrix is 120-200mm, the translational speed of spray gun is controlled
For 300-800mm/min；Electric current 400A, voltage 50KV, powder sending quantity 40gmin-1, powder feeding throughput 4Lmin-1, main gas class
Type Ar；This gas type hydrogen, primary air amount 40Lmin-1, secondary throughput 5Lmin-1, main atmospheric pressure 8MPa, secondary atmospheric pressure
6MPa；During the use plasma spray coating process sprays zirconia coating on spraying matrix, the spraying matrix surface
Cooled down with compressed air stream, the surface temperature control of the spraying matrix is no more than 200 DEG C.
2. preparation method according to claim 1, it is characterised in that the preparation of the zirconium oxide spray coating powder includes：With matter
Percentages are measured, after 93-98% Zirconium oxide powder is mixed with 2-7% carbon dust, in 1500-1700 DEG C of hydrogen atmosphere
Sintering 6-10 hours, it is then spray-dried, obtain the zirconium oxide spray coating powder of 100-400 mesh.
3. preparation method according to claim 2, it is characterised in that：The purity of the Zirconium oxide powder is not less than
99.5wt%, particle diameter is 1-5um.
4. preparation method according to claim 1, it is characterised in that the processing of the spraying matrix includes：First clean, beat
The oil stain and oxide layer except the spraying matrix surface are ground off, the spraying matrix surface is then roughened using sandblasting.
5. preparation method according to claim 1, it is characterised in that：The spraying prime coat is in spraying matrix surface spray
Apply 0.1-0.3mm alloy coat.
6. preparation method according to claim 5, it is characterised in that：The spraying alloy coat is to use plasma spray
Coating is in the spraying matrix surface spraying nickel alclad, nickel chromium triangle, nickel chromium triangle aluminium or nichrome-chromium-aluminium-yttrium powder, or uses arc process described
Spray matrix surface spraying aluminium bronze or ni-al alloyed wire.
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| CN104831242B (en) * | 2015-04-08 | 2017-11-24 | 无锡舒玛天科新能源技术有限公司 | Large scale integration aluminium neodymium rotary target material and preparation method thereof |
| CN104805406B (en) * | 2015-04-17 | 2017-06-06 | 无锡舒玛天科新能源技术有限公司 | Aluminium scandium rotary target material and preparation method thereof |
| CN104831244A (en) * | 2015-04-17 | 2015-08-12 | 无锡舒玛天科新能源技术有限公司 | Aluminum tantalum rotating target material, and method used for preparing aluminum tantalum rotating target material via controlled atmosphere cold spraying |
| CN105058923A (en) * | 2015-08-17 | 2015-11-18 | 基迈克材料科技（苏州）有限公司 | Sputtering target capable of enhancing wear resistance and corrosion resistance of coated glass and manufacturing method |
| EP3184663B1 (en) | 2015-12-23 | 2020-04-15 | Materion Advanced Materials Germany GmbH | Zirconium oxide based sputtering target |
| CN106893992A (en) * | 2017-03-01 | 2017-06-27 | 芜湖映日科技有限公司 | A kind of method for spraying the recycling of target matrix |
| CN108707870A (en) * | 2018-05-24 | 2018-10-26 | 宁波森利电子材料有限公司 | The preparation method of the sial rotary target material of high-compactness |
| CN111041432A (en) * | 2019-11-26 | 2020-04-21 | 广州市尤特新材料有限公司 | Rotary zirconia target material and preparation method thereof |
| CN115096675B (en) * | 2022-06-07 | 2023-08-11 | 佛山科学技术学院 | Zirconium tube calibration sample for underwater vortex detection and preparation method thereof |
| CN114990486B (en) * | 2022-07-28 | 2022-10-18 | 广州市尤特新材料有限公司 | Rotary zirconia target material and preparation method thereof |
| CN115894034A (en) * | 2022-12-08 | 2023-04-04 | 北京航空航天大学 | Preparation method of chromium aluminum carbide ceramic, chromium aluminum carbide ceramic and application |
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| US5354446A (en) * | 1988-03-03 | 1994-10-11 | Asahi Glass Company Ltd. | Ceramic rotatable magnetron sputtering cathode target and process for its production |
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| CN103045995A (en) * | 2012-12-19 | 2013-04-17 | 西北稀有金属材料研究院 | Rotary niobium oxide target material and preparation method thereof |
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| CN102286717B (en) * | 2011-09-01 | 2013-07-03 | 基迈克材料科技（苏州）有限公司 | Cylindrical large-area film coating target prepared through plasma spray coating and method |
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| US5354446A (en) * | 1988-03-03 | 1994-10-11 | Asahi Glass Company Ltd. | Ceramic rotatable magnetron sputtering cathode target and process for its production |
| EP0852266A1 (en) * | 1995-08-23 | 1998-07-08 | Asahi Glass Company Ltd. | Target, process for production thereof, and method of forming highly refractive film |
| CN103045995A (en) * | 2012-12-19 | 2013-04-17 | 西北稀有金属材料研究院 | Rotary niobium oxide target material and preparation method thereof |
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