WO2012020662A1 - タンタルスパッタリングターゲット - Google Patents
タンタルスパッタリングターゲット Download PDFInfo
- Publication number
- WO2012020662A1 WO2012020662A1 PCT/JP2011/067651 JP2011067651W WO2012020662A1 WO 2012020662 A1 WO2012020662 A1 WO 2012020662A1 JP 2011067651 W JP2011067651 W JP 2011067651W WO 2012020662 A1 WO2012020662 A1 WO 2012020662A1
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- WIPO (PCT)
- Prior art keywords
- oxygen
- tantalum
- crystal grain
- grain size
- target
- Prior art date
Links
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 62
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000013078 crystal Substances 0.000 claims abstract description 68
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 67
- 239000001301 oxygen Substances 0.000 claims abstract description 67
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 67
- 238000005477 sputtering target Methods 0.000 claims abstract description 27
- 239000007789 gas Substances 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 abstract description 3
- 238000001953 recrystallisation Methods 0.000 description 26
- 238000009826 distribution Methods 0.000 description 24
- 238000000137 annealing Methods 0.000 description 22
- 238000004544 sputter deposition Methods 0.000 description 21
- 239000000463 material Substances 0.000 description 16
- 230000006641 stabilisation Effects 0.000 description 12
- 238000011105 stabilization Methods 0.000 description 12
- 238000005242 forging Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 10
- 239000002994 raw material Substances 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 238000010894 electron beam technology Methods 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- 238000005096 rolling process Methods 0.000 description 7
- 239000013077 target material Substances 0.000 description 7
- 238000005482 strain hardening Methods 0.000 description 6
- 238000010273 cold forging Methods 0.000 description 5
- 238000005204 segregation Methods 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 238000004904 shortening Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052752 metalloid Inorganic materials 0.000 description 2
- 150000002738 metalloids Chemical class 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005097 cold rolling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 150000003481 tantalum Chemical class 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/22—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
- B21B1/24—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length in a continuous or semi-continuous process
- B21B1/28—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length in a continuous or semi-continuous process by cold-rolling, e.g. Steckel cold mill
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
-
- 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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/028—Physical treatment to alter the texture of the substrate surface, e.g. grinding, polishing
-
- 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
- C23C14/14—Metallic material, boron or silicon
-
- 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
Definitions
- the present invention relates to a high-purity tantalum sputtering target having a uniform and fine structure, stable plasma, and excellent film uniformity (uniformity).
- sputtering that forms a coating of metal or ceramic material has been used in many fields such as electronics, corrosion-resistant materials and decoration, catalysts, and production of cutting / polishing materials and wear-resistant materials.
- the sputtering method itself is a well-known method in the above field, but recently, particularly in the field of electronics, tantalum sputtering suitable for forming a complex-shaped film, forming a circuit, or forming a barrier film. A target is requested.
- this tantalum target is processed into a target by repeatedly hot forging and annealing (heat treatment) of an ingot or billet obtained by melting and casting a tantalum raw material, and further rolling and finishing (machine, polishing, etc.). .
- hot forging of an ingot or billet destroys the cast structure, diffuses and disappears pores and segregation, and further recrystallizes by annealing to increase the density and strength of the structure. It is manufactured by.
- a melt-cast ingot or billet has a crystal grain size of 50 mm or more.
- the cast structure is destroyed by hot forging and recrystallization annealing of an ingot or billet, and generally uniform and fine crystal grains (100 ⁇ m or less) are obtained.
- high-purity Ta target for forming a TaN film used as a barrier layer for a Cu wiring film contains 0.001 to 20 ppm of an element selected from Ag, Au and Cu as elements having self-sustaining discharge characteristics Further, high-purity Ta is used in which the total amount of Fe, Ni, Cr, Si, Al, Na, and K as impurity elements is 100 ppm or less, and the value obtained by subtracting these is in the range of 99.99 to 99.999%. (See Patent Document 3). As far as these patent documents are viewed, the inclusion of a specific element does not refine the structure and thereby stabilize the plasma.
- Patent Document 3 by adding 0.001 to 20 ppm of an element selected from Ag, Au, and Cu, the addition of a trace amount of elements up to 0.001 ppm increases the amount of released Ta ions.
- the contents of Mo, W, Ge, and Co are permitted to be 10 ppm, 20 ppm, 10 ppm, and less than 10 ppm, respectively. This alone has impurities of less than 50 ppm.
- the present invention maintains high purity of tantalum, and by adding a specific element, it has a uniform fine structure, plasma is stable, and high purity with excellent film uniformity (uniformity) It is an object to provide a tantalum sputtering target.
- the present invention maintains a high purity of tantalum, and by adding a specific element, it has a uniform fine structure, plasma is stable, and film uniformity
- the knowledge that a high purity tantalum sputtering target excellent in (uniformity) can be obtained was obtained.
- the present invention is based on this finding.
- the tantalum sputtering target characterized in that the purity is 99.998% or more 4)
- the variation in oxygen content in the target is ⁇ 20% or less, in any one of 1) to 3) above
- the crystal grain size variation is ⁇ 20% or less
- the present invention maintains a high purity of tantalum, and by adding oxygen as an essential component, it has a uniform and fine structure, plasma is stable, and excellent in film uniformity (uniformity). It has the outstanding effect that a purity tantalum sputtering target can be provided. In addition, plasma stabilization during sputtering is stabilized even in the initial stage, so that the burn-in time can be shortened.
- High purity tantalum is used as a raw material for the tantalum (Ta) target used in the present invention.
- Examples of this high-purity tantalum are shown in Table 1 (see Japan Invention Association, published technical report 2005-502770, published technical report name “high-purity tantalum and sputtering target comprising high-purity tantalum”).
- Table 2 all impurities are less than 1 mass ppm except for gas components. That is, it is 99.999 to 99.9999 mass%, but such high-purity tantalum can be used.
- the sputtering target of the present invention is usually produced by the following steps.
- tantalum for example, 4N (99.99% or more) high-purity tantalum is used, and an appropriate amount of oxygen (O) is added thereto as a target raw material.
- This is melted and purified by electron beam melting or the like to increase purity, and this is cast to produce an ingot or billet.
- 99.999 to 99.9999 mass% high-purity tantalum shown in Table 2 can be used from the beginning.
- the ingot or billet is subjected to a series of processing such as annealing-forging, rolling, annealing (heat treatment), finishing, and the like.
- first time cold forging
- second time Cold forging (second time)-Recrystallization annealing temperature between recrystallization start temperature and 1673K
- third time -Cold (hot) rolling
- the cast structure By forging or rolling, the cast structure can be destroyed, and the pores and segregation can be diffused or disappeared. Furthermore, this can be recrystallized by annealing, and this cold forging or cold rolling and recrystallization annealing can be repeated. , The densification, refinement and strength of the structure can be increased.
- the recrystallization annealing may be performed once, but the defects on the structure can be reduced as much as possible by repeating twice. Further, the cold (hot) rolling and the recrystallization annealing between the recrystallization start temperature and 1373 K may be repeated or may be one cycle. Thereafter, a final target shape is finished by finishing such as machining and polishing.
- a tantalum target is manufactured by the above manufacturing process, but this manufacturing process shows an example, and the present invention does not invent this manufacturing process.
- the present invention includes all of them.
- a material with a purity level of 6N is often used, but there is a drawback that the crystal grains of the target are apt to be coarsened.
- the present inventors usually have a crystal grain size locally in a portion where oxygen having a content of about 20 massppm happens to be segregated to about 50 massppm. I found that it was miniaturized. From this, a hint was obtained that the addition of oxygen would be effective for miniaturization of the tantalum target, and this led to the present invention.
- tantalum sputtering target of the present invention it is important that tantalum having a purity excluding oxygen and gas components of 99.998% or more contains oxygen of 30 mass ppm or more and 100 mass ppm or less as an essential component.
- oxygen exists as a solid solution (interstitial solid solution).
- the lower limit value of 30 massppm for oxygen is a numerical value for exerting an effect
- the upper limit value for oxygen of 100 massppm is an upper limit value for maintaining the effect of the present invention.
- 100 mass ppm of oxygen is set as the upper limit.
- the inclusion of oxygen in the tantalum forms a uniform fine structure of the target, thereby stabilizing the plasma, thereby improving the uniformity of the sputtering film.
- the burn-in time can be shortened.
- the purity of tantalum needs to be high, that is, 99.998% or higher.
- gas components such as oxygen, hydrogen, carbon and nitrogen having a small atomic radius can be excluded.
- the gas component is difficult to remove unless it is a special method, and it is difficult to remove at the time of purification in a normal production process. Therefore, the gas component is excluded from the purity of the tantalum of the present invention.
- oxygen produces a uniform fine structure of tantalum, but mixing of other metal components, metalloids (metalloids), oxides, nitrides, carbides, and other ceramics is detrimental and acceptable. Can not. This is because these impurities are considered to suppress the action of oxygen. Further, these impurities are clearly different from oxygen, and it is difficult to finish the crystal grain size of the tantalum target uniformly, and do not contribute to stabilization of sputtering characteristics.
- the tantalum sputtering target of the present invention contains 40 massppm or more and 100 massppm or less of oxygen as an essential component, and the purity excluding oxygen and gas components is 99.998% or more. Furthermore, it is a tantalum sputtering target containing oxygen as an essential component in an amount of 40 massppm or more and 70 massppm or less and having a purity excluding oxygen and gas components of 99.998% or more.
- metallic impurities other than gas components include Mg, Al, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Nb, Mo, Sn, W, and U. It is desirable to set it to 1 ppm or less.
- the variation in oxygen content in the target is ⁇ 20% or less.
- the proper oxygen content has the function (property) to form a uniform fine structure of the tantalum sputtering target
- the more uniform dispersion of oxygen contributes more strongly to the uniform fine structure of the target structure. be able to.
- these can be easily achieved in a normal manufacturing process, but it is necessary to keep in mind that the variation in the oxygen content of the target is ⁇ 20% or less, and clearly have the intention.
- the variation in the oxygen content of this target for example, in the case of a disk-shaped target, three points (center point, half point of radius, outer circumference or its circumference) on eight equal lines passing through the center of the disk. Neighboring points) are taken, and the oxygen content of a total of 17 points ⁇ 16 points + center point (one point because the center point is common) ⁇ is analyzed. At each point, the variation can be calculated based on the equation ⁇ (maximum value ⁇ minimum value) / (maximum value + minimum value) ⁇ ⁇ 100.
- the tantalum sputtering target of the present invention preferably has an average crystal grain size of 120 ⁇ m or less.
- the crystal grain size can be made finer by appropriate addition of oxygen and the normal manufacturing process, but it is necessary to pay attention to the fact that the average crystal grain size is 120 ⁇ m or less, and to clearly have the intention. . Further, it is more desirable that the variation in the crystal grain size is ⁇ 20% or less.
- the variation in the average crystal grain size for example, in the case of a disk-shaped target, three points (center point, half point of radius, outer periphery or its neighboring points) on eight equal lines passing through the center of the disk. ), And measure the crystal grain size of the oxide of a total of 17 points ⁇ 16 points + center point (one point because the center point is common) ⁇ . At each point, the variation in crystal grain size can be calculated based on the formula ⁇ (maximum value ⁇ minimum value) / (maximum value + minimum value) ⁇ ⁇ 100.
- plasma is stable and film uniformity (uniformity) is excellent.
- plasma stabilization at the time of sputtering is stabilized even at an initial stage, and thus has an effect of shortening the burn-in time.
- Example 1 A raw material obtained by adding an equivalent of 30 massppm of oxygen to tantalum having a purity of 99.998% was melted by electron beam, and cast into an ingot having a thickness of 200 mm and a diameter of 200 mm ⁇ .
- this ingot or billet was forged at room temperature and then recrystallized and annealed at a temperature of 1500K.
- a material having a structure with an average crystal grain size of 200 ⁇ m and a thickness of 120 mm and a diameter of 130 mm was obtained. This corresponds to the annealing (first time) at a temperature of ingot-forge-stretching-1373K to 1673K described in the above paragraph [0015].
- the following examples and comparative examples can be similarly handled.
- the sheet resistance depends on the film thickness
- the distribution of the sheet resistance in the wafer (12 inches) was measured, thereby examining the distribution of the film thickness. Specifically, the sheet resistance at 49 points on the wafer was measured, and the standard deviation ( ⁇ ) was calculated.
- Table 2 As is apparent from Table 2, in this example, the variation in the resistance distribution in the sheet is small (2.4 to 3.1%) from the initial stage to the late stage of sputtering, that is, the variation in the film thickness distribution is small. Yes.
- Example 2 A raw material in which oxygen equivalent to 50 massppm was added to tantalum having a purity of 99.998% was melted by electron beam and cast into an ingot having a thickness of 200 mm and a diameter of 200 mm ⁇ .
- the crystal grain size in this case was about 45 mm.
- the ingot or billet was forged at room temperature and then recrystallized and annealed at a temperature of 1500K. As a result, a material having a structure with an average crystal grain size of 200 ⁇ m and a thickness of 120 mm and a diameter of 130 mm was obtained.
- the intermediate and final cold working and recrystallization annealing were adjusted so as to have the following average crystal grain size and crystal grain size variation.
- the average crystal grain size and variation vary depending on the amount of oxygen added, but in the present embodiment, these adjustments were possible.
- the average crystal grain size of the target was 70 ⁇ m, and the variation in crystal grain size was ⁇ 16%. Moreover, the variation in oxygen content was ⁇ 14%.
- the results are also shown in Table 2.
- Example 3 A raw material obtained by adding an equivalent of 70 massppm of oxygen to tantalum having a purity of 99.998% was melted by electron beam, and cast into an ingot having a thickness of 200 mm and a diameter of 200 mm ⁇ .
- this ingot or billet was forged at room temperature and then recrystallized and annealed at a temperature of 1500K. As a result, a material having a structure with an average crystal grain size of 200 ⁇ m and a thickness of 120 mm and a diameter of 130 mm was obtained.
- the forging and heat treatment were repeated again to obtain a material having a structure with an average crystal grain size of 80 ⁇ m and a thickness of 120 mm and a diameter of 130 mm ⁇ .
- the intermediate and final cold working and recrystallization annealing were adjusted so as to have the following average crystal grain size and crystal grain size variation.
- the average crystal grain size and variation vary depending on the amount of oxygen added, but in the present embodiment, these adjustments were possible.
- the average crystal grain size of the target was 50 ⁇ m, and the variation of the crystal grain size was ⁇ 12%. Moreover, the variation in oxygen content was ⁇ 18%.
- the results are also shown in Table 2.
- Example 4 A raw material obtained by adding an equivalent of 100 massppm of oxygen to tantalum having a purity of 99.998% was melted by electron beam, and cast into an ingot having a thickness of 200 mm and a diameter of 200 mm ⁇ .
- this ingot or billet was forged at room temperature and then recrystallized and annealed at a temperature of 1500K. As a result, a material having a structure with an average crystal grain size of 200 ⁇ m and a thickness of 120 mm and a diameter of 130 mm was obtained.
- the forging and heat treatment were repeated again to obtain a material having a structure with an average crystal grain size of 70 ⁇ m and a thickness of 120 mm and a diameter of 130 mm ⁇ .
- the intermediate and final cold working and recrystallization annealing were adjusted so as to have the following average crystal grain size and crystal grain size variation.
- the average crystal grain size and variation vary depending on the amount of oxygen added, but in the present embodiment, these adjustments were possible.
- the average crystal grain size of the target was 30 ⁇ m, and the variation of the crystal grain size was ⁇ 7%. Moreover, the variation in oxygen content was ⁇ 16%.
- the results are also shown in Table 2.
- the ingot or billet was forged at room temperature and then recrystallized and annealed at a temperature of 1500K. As a result, a material having a structure with an average crystal grain size of 200 ⁇ m and a thickness of 120 mm and a diameter of 130 mm was obtained.
- the forging and heat treatment were repeated again to obtain a material having a structure with an average crystal grain size of 100 ⁇ m and a thickness of 120 mm and a diameter of 130 mm ⁇ .
- the middle and final cold working and recrystallization annealing were adjusted so as to have an appropriate average crystal grain size and variation in crystal grain size, but in this comparative example, the variation in crystal grain size could not be adjusted, and the target The average crystal grain size was 130 ⁇ m, and the variation in crystal grain size was ⁇ 35%. Moreover, the variation in oxygen content was ⁇ 15%.
- Table 2 The results are also shown in Table 2.
- the sheet resistance depends on the film thickness
- the distribution of the sheet resistance in the wafer (12 inches) was measured, thereby examining the distribution of the film thickness. Specifically, the sheet resistance at 49 points on the wafer was measured, and the standard deviation ( ⁇ ) was calculated. The results are also shown in Table 2. As is apparent from Table 2, in this example, the variation in the resistance distribution in the sheet is large (3.7 to 5.8%) from the initial stage to the late stage, that is, the fluctuation in the film thickness distribution is large. It was.
- the ingot or billet was forged at room temperature and then recrystallized and annealed at a temperature of 1500K. As a result, a material having a structure with an average crystal grain size of 190 ⁇ m and a thickness of 120 mm and a diameter of 130 mm was obtained.
- the intermediate and final cold working and recrystallization annealing were adjusted so as to have an appropriate average crystal grain size and variation in crystal grain size, but in this comparative example, these adjustments could not be made, and the average crystal grain of the target Although the diameter was 15 ⁇ m, the crystal grain size variation was ⁇ 50% due to non-recrystallization, and the variation was large. Moreover, the variation in oxygen content was ⁇ 60%. The results are also shown in Table 2.
- the sheet resistance depends on the film thickness
- the distribution of the sheet resistance in the wafer (12 inches) was measured, thereby examining the distribution of the film thickness. Specifically, the sheet resistance at 49 points on the wafer was measured, and the standard deviation ( ⁇ ) was calculated.
- Table 2 As is apparent from Table 2, in this example, the variation in the resistance distribution in the sheet is large (4.8 to 7.2%) from the initial stage to the late stage of sputtering, that is, the variation in the film thickness distribution is large. It was.
- oxygen is contained in an amount of 30 massppm or more and 100 massppm or less as an essential component, and the purity excluding oxygen and gas components is 99.998% or more. It has an excellent effect that a high-purity tantalum sputtering target that is stable and excellent in film uniformity (uniformity) can be provided. In addition, since plasma stabilization during sputtering is stabilized even in the initial stage, it has the effect of shortening the burn-in time, so that it has the effect of shortening the burn-in time. It is useful as a target suitable for formation.
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Abstract
Description
スパッタリング法自体は上記の分野で、よく知られた方法であるが、最近では、特にエレクトロニクスの分野において、複雑な形状の被膜の形成や回路の形成、あるいはバリア膜の形成等に適合するタンタルスパッタリングターゲットが要求されている。
このような製造工程において、インゴット又はビレットの熱間鍛造は、鋳造組織を破壊し、気孔や偏析を拡散、消失させ、さらにこれを焼鈍することにより再結晶化し、組織の緻密化と強度を高めることによって製造されている。
一般に、溶解鋳造されたインゴット又はビレットは、50mm以上の結晶粒径を有している。そして、インゴット又はビレットの熱間鍛造と再結晶焼鈍により、鋳造組織が破壊され、おおむね均一かつ微細な(100μm以下の)結晶粒が得られる。
そのため、ターゲットの製造工程において、再結晶組織の微細化と均一化、さらには特定の結晶方位に揃えようとする方策が採られている(例えば、特許文献1及び特許文献2参照)。
これらの特許文献を見る限り、特定の元素の含有が、組織を微細化させ、これによってプラズマを安定化させるということは行われていない。
しかも、特許文献3の表2に示すように、Mo、W、Ge、Co量は、それぞれ10ppm、20ppm、10ppm、10ppm未満の含有が許容されている。これだけでも50ppm未満の不純物がある。
これは、従来の高純度タンタルのレベル以下であり、高純度タンタルの特性を活かすことはできないことが強く予想される。
本発明は、この知見に基づいて、
1)30massppm以上、100massppm以下の酸素を必須成分として含有し、酸素及びガス成分を除く純度が99.998%以上であることを特徴とするタンタルスパッタリングターゲット
2)40massppm以上、100massppm以下の酸素を必須成分として含有し、酸素及びガス成分を除く純度が99.998%以上であることを特徴とするタンタルスパッタリングターゲット
3)酸素を40massppm以上、70massppm以下を必須成分として含有し、酸素及びガス成分を除く純度が99.998%以上であることを特徴とするタンタルスパッタリングターゲット
4)ターゲット中の酸素含有量のばらつきが±20%以下であることを特徴とする上記1)~3)のいずれかに記載のタンタルスパッタリングターゲット
5)平均結晶粒径が120μm以下であることを特徴とする上記1)~4)のいずれかに記載のタンタルスパッタリングターゲット
6)結晶粒径のばらつきが±20%以下であることを特徴とする上記5)記載のタンタルスパッタリングターゲット、を提供する。
この表2では、ガス成分を除き、全ての不純物は1massppm未満である。すなわち99.999~99.9999mass%となっているが、このような高純度タンタルを使用することができる。
その一例を示すと、まずタンタル、例えば4N(99.99%以上)の高純度タンタルを使用し、これに酸素(O)を適量添加してターゲットの原料とする。これを電子ビーム溶解等により溶解・精製して純度を高め、これを鋳造してインゴット又はビレットを作製する。当然ながら、最初から表2に示す99.999~99.9999mass%高純度タンタルを使用することもできる。
次に、このインゴット又はビレットを焼鈍-鍛造、圧延、焼鈍(熱処理)、仕上げ加工等の一連の加工を行う。
タンタルターゲットの特性を活かすために、6Nレベルの純度の材料を使用することが多いが、どうしてもターゲットの結晶粒が粗大化し易いという欠点があった。
本発明者らは、このような6Nレベルのターゲットの製造工程において、通常であれば20massppm程度の含有量である酸素が、たまたま50massppm程度に偏析していた部分で、結晶粒径が局所的に微細化していることを発見した。このことから、酸素の添加がタンタルターゲットの微細化に有効ではないかというヒントを得、これが本願発明につながる契機となった。
本発明のタンタルスパッタリングターゲットにおいて、酸素は固溶体(侵入型固溶体)として存在する。上記酸素の下限値30massppmは効果を発揮させるための数値であり、酸素の上限値100massppmは、本発明の効果を持続させるための上限値である。この上限値を超える場合には、酸素の偏析が起こり、酸素の一部未再結晶部が発生し、結果としてバーンインが長くなるので、酸素100massppmを上限値とする。
この場合、タンタルの純度は、高純度すなわち99.998%以上とする必要がある。この場合、原子半径の小さい、酸素、水素、炭素、窒素等のガス成分は除外することができる。一般にガス成分は特殊な方法でなければ除去は困難であり、通常の生産工程で精製の際に除去することは難しいので、ガス成分は本願発明のタンタルの純度からは除外する。
さらに、酸素を40massppm以上、70massppm以下を必須成分として含有し、酸素及びガス成分を除く純度が99.998%以上のタンタルスパッタリングターゲットである。
ガス成分以外の金属の不純物の例としては、Mg、Al、Ca、Ti、Cr、Mn、Fe、Ni、Cu、Nb、Mo、Sn、W、Uを挙げることができるが、これらはいずれも1ppm以下とすることが望ましい。
適度な酸素の含有がタンタルスパッタリングターゲットの均一微細な組織を形成する機能(性質)を有する以上、酸素はより均一に分散していることは、ターゲット組織の均一微細な組織に、より強く貢献させことができる。
当然ながら、通常の製造工程において、これらは容易に達成できるのであるが、ターゲットの酸素含有量のばらつきを±20%以下とする点に留意し、その意図を明確に持つことが必要である。
そして、各点において、{(最大値-最小値)/(最大値+最小値)}×100の式に基づいて、ばらつきを計算することができる。
本発明のタンタルスパッタリングターゲットは、さらに平均結晶粒径が120μm以下であることが望ましい。酸素の適度な添加と通常の製造工程において、結晶粒径の微細化が達成できるのであるが、平均結晶粒径が120μm以下とする点に留意し、その意図を明確に持つことが必要である。
また、この結晶粒径のばらつきが±20%以下とすることがより望ましい。
純度99.998%のタンタルに酸素30massppm相当量を添加した原料を電子ビーム溶解し、これを鋳造して厚さ200mm、直径200mmφのインゴットとした。この場合の結晶粒径は約50mmであった。
次に、このインゴット又はビレットを室温で鍛伸した後、1500Kの温度で再結晶焼鈍した。これによって平均結晶粒径が200μmの組織を持つ厚さ120mm、直径130mmφの材料が得られた。これは、上記段落[0015]に記載したインゴット-鍛伸-1373K~1673Kの温度での焼鈍(1回目)に対応する。以下の実施例、比較例においても同様に対応させることができる。
そして鍛造、熱処理を再度繰り返した。これは、上記段落[0015]に記載した冷間鍛造(2回目)-再結晶開始温度~1673Kの間での再結晶焼鈍(3回目)に対応する。以下の実施例、比較例においても同様に対応させることができる。
これによって平均結晶粒径が100μmの組織を持つ厚さ120mm、直径130mmφの材料を得た。
途中及び最後の冷間加工並びに再結晶焼鈍は、以下の平均結晶粒径及び結晶粒径のばらつきとなるように調節した。なお、この平均結晶粒径とばらつきは、酸素の添加量によっても変化するが、本実施例では、これらの調節が可能であった。
ターゲットの平均結晶粒径は85μmであり、結晶粒径のばらつきは±17%であった。また、酸素含有量のばらつきは±15%であった。この結果を、表2に示す。
その結果を、同様に表2に示す。表2から明らかなように、本実施例においては、スパッタ初期から後期にかけてシート内抵抗分布の変動が少ない(2.4~3.1%)、すなわち膜厚分布の変動が少ないことを示している。
純度99.998%のタンタルに酸素50massppm相当量を添加した原料を電子ビーム溶解し、これを鋳造して厚さ200mm、直径200mmφのインゴットとした。この場合の結晶粒径は約45mmであった。
鍛造、熱処理を再度繰り返し、これによって平均結晶粒径が90μmの組織を持つ厚さ120mm、直径130mmφの材料を得た。
ターゲットの平均結晶粒径は70μmであり、結晶粒径のばらつきは±16%であった。また、酸素含有量のばらつきは±14%であった。この結果を、同様に表2に示す。
その結果を、同様に表2に示す。表2から明らかなように、本実施例においては、スパッタ初期から後期にかけてシート内抵抗分布の変動が少ない(2.1~2.6%)、すなわち膜厚分布の変動が少ないことを示している。
純度99.998%のタンタルに酸素70massppm相当量を添加した原料を電子ビーム溶解し、これを鋳造して厚さ200mm、直径200mmφのインゴットとした。この場合の結晶粒径は約40mmであった。
次に、このインゴット又はビレットを室温で鍛伸した後、1500Kの温度で再結晶焼鈍した。これによって平均結晶粒径が200μmの組織を持つ厚さ120mm、直径130mmφの材料が得られた。
ターゲットの平均結晶粒径は50μmであり、結晶粒径のばらつきは±12%であった。また、酸素含有量のばらつきは±18%であった。この結果を、同様に表2に示す。
その結果を、同様に表2に示す。表2から明らかなように、本実施例においては、スパッタ初期から後期にかけてシート内抵抗分布の変動が少ない(1.5~1.8%)、すなわち膜厚分布の変動が少ないことを示している。
純度99.998%のタンタルに酸素100massppm相当量を添加した原料を電子ビーム溶解し、これを鋳造して厚さ200mm、直径200mmφのインゴットとした。この場合の結晶粒径は約35mmであった。
次に、このインゴット又はビレットを室温で鍛伸した後、1500Kの温度で再結晶焼鈍した。これによって平均結晶粒径が200μmの組織を持つ厚さ120mm、直径130mmφの材料が得られた。
ターゲットの平均結晶粒径は30μmであり、結晶粒径のばらつきは±7%であった。また、酸素含有量のばらつきは±16%であった。この結果を、同様に表2に示す。
その結果を、同様に表2に示す。表2から明らかなように、本実施例においては、スパッタ初期から後期にかけてシート内抵抗分布の変動が少ない(2.2~3.5%)、すなわち膜厚分布の変動が少ないことを示している。
純度99.995%のタンタルに酸素20massppm相当量を添加した原料を電子ビーム溶解し、これを鋳造して厚さ200mm、直径200mmφのインゴットとした。この場合の結晶粒径は約60mmであった。
その結果を、同様に表2に示す。表2から明らかなように、本実施例においては、スパッタ初期から後期にかけてシート内抵抗分布の変動が大きく(3.7~5.8%)、すなわち膜厚分布の変動が大きくなることを示していた。
純度99.999%のタンタルに酸素150massppm相当量を添加した原料を電子ビーム溶解し、これを鋳造して厚さ200mm、直径200mmφのインゴットとした。この場合の結晶粒径は約20mmであった。
その結果を、同様に表2に示す。表2から明らかなように、本実施例においては、スパッタ初期から後期にかけてシート内抵抗分布の変動が大きく(4.8~7.2%)、すなわち膜厚分布の変動が大きくなることを示していた。
Claims (6)
- 30massppm以上、100massppm以下の酸素を必須成分として含有し、酸素及びガス成分を除く純度が99.998%以上であることを特徴とするタンタルスパッタリングターゲット。
- 40massppm以上、100massppm以下の酸素を必須成分として含有し、酸素及びガス成分を除く純度が99.998%以上であることを特徴とするタンタルスパッタリングターゲット。
- 酸素を40massppm以上、70massppm以下を必須成分として含有し、酸素及びガス成分を除く純度が99.998%以上であることを特徴とするタンタルスパッタリングターゲット。
- ターゲット中の酸素含有量のばらつきが±20%以下であることを特徴とする請求項1~3のいずれか一項に記載のタンタルスパッタリングターゲット。
- 平均結晶粒径が120μm以下であることを特徴とする請求項1~4のいずれか一項に記載のタンタルスパッタリングターゲット。
- 結晶粒径のばらつきが±20%以下であることを特徴とする請求項5記載のタンタルスパッタリングターゲット。
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Cited By (2)
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WO2015050041A1 (ja) * | 2013-10-01 | 2015-04-09 | Jx日鉱日石金属株式会社 | タンタルスパッタリングターゲット |
EP2913423A1 (en) * | 2013-03-04 | 2015-09-02 | JX Nippon Mining & Metals Corporation | Tantalum sputtering target and production method therefor |
Families Citing this family (9)
Publication number | Priority date | Publication date | Assignee | Title |
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SG173141A1 (en) | 2009-05-22 | 2011-08-29 | Jx Nippon Mining & Metals Corp | Tantalum sputtering target |
US9845528B2 (en) | 2009-08-11 | 2017-12-19 | Jx Nippon Mining & Metals Corporation | Tantalum sputtering target |
KR20130008089A (ko) | 2010-08-09 | 2013-01-21 | 제이엑스 닛코 닛세키 킨조쿠 가부시키가이샤 | 탄탈 스퍼터링 타깃 |
JP5324016B1 (ja) | 2012-03-21 | 2013-10-23 | Jx日鉱日石金属株式会社 | タンタルスパッタリングターゲット及びその製造方法並びに同ターゲットを用いて形成した半導体配線用バリア膜 |
SG11201501370PA (en) | 2012-12-19 | 2015-04-29 | Jx Nippon Mining & Metals Corp | Tantalum sputtering target and method for producing same |
WO2014097897A1 (ja) | 2012-12-19 | 2014-06-26 | Jx日鉱日石金属株式会社 | タンタルスパッタリングターゲット及びその製造方法 |
JP5897767B2 (ja) | 2013-11-06 | 2016-03-30 | Jx金属株式会社 | スパッタリングターゲット/バッキングプレート組立体 |
US10658163B2 (en) | 2015-05-22 | 2020-05-19 | Jx Nippon Mining & Metals Corporation | Tantalum sputtering target, and production method therefor |
JP6293928B2 (ja) | 2015-05-22 | 2018-03-14 | Jx金属株式会社 | タンタルスパッタリングターゲット及びその製造方法 |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2001020065A (ja) * | 1999-07-07 | 2001-01-23 | Hitachi Metals Ltd | スパッタリング用ターゲット及びその製造方法ならびに高融点金属粉末材料 |
US6331233B1 (en) | 2000-02-02 | 2001-12-18 | Honeywell International Inc. | Tantalum sputtering target with fine grains and uniform texture and method of manufacture |
JP2002060934A (ja) | 2000-08-24 | 2002-02-28 | Toshiba Corp | スパッタリングターゲット |
JP2002518593A (ja) | 1998-06-17 | 2002-06-25 | ジヨンソン マテイ エレクトロニクス,インコーポレーテツド | 微細で一様な構造とテキスチュアを有する金属製品及びその製造方法 |
JP2002363662A (ja) * | 2001-06-01 | 2002-12-18 | Nikko Materials Co Ltd | 高純度タンタルの回収方法並びに高純度タンタルスパッタリングターゲット及び該スパッタリングターゲットにより形成された薄膜 |
WO2010134417A1 (ja) * | 2009-05-22 | 2010-11-25 | Jx日鉱日石金属株式会社 | タンタルスパッタリングターゲット |
WO2011018971A1 (ja) * | 2009-08-11 | 2011-02-17 | Jx日鉱日石金属株式会社 | タンタルスパッタリングターゲット |
WO2011018970A1 (ja) * | 2009-08-11 | 2011-02-17 | Jx日鉱日石金属株式会社 | タンタルスパッタリングターゲット |
Family Cites Families (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH1180942A (ja) * | 1997-09-10 | 1999-03-26 | Japan Energy Corp | Taスパッタターゲットとその製造方法及び組立体 |
JP2001073125A (ja) * | 1999-09-08 | 2001-03-21 | Nikko Materials Co Ltd | Co−Ta系合金スパッタリングターゲット及びその製造方法 |
JP2001316806A (ja) * | 2000-05-08 | 2001-11-16 | Hitachi Metals Ltd | 高純度Alターゲットおよび配線膜 |
TWI341337B (en) * | 2003-01-07 | 2011-05-01 | Cabot Corp | Powder metallurgy sputtering targets and methods of producing same |
WO2006001976A2 (en) * | 2004-06-15 | 2006-01-05 | Tosoh Smd, Inc. | High purity target manufacturing methods |
US7998287B2 (en) * | 2005-02-10 | 2011-08-16 | Cabot Corporation | Tantalum sputtering target and method of fabrication |
JP4619811B2 (ja) * | 2005-02-16 | 2011-01-26 | 株式会社東芝 | スパッタリングターゲット、高屈折率膜とその製造方法、およびそれを用いた反射防止膜とディスプレイ装置 |
JP4949259B2 (ja) * | 2005-10-04 | 2012-06-06 | Jx日鉱日石金属株式会社 | スパッタリングターゲット |
JP4719174B2 (ja) * | 2007-03-22 | 2011-07-06 | 株式会社東芝 | スパッタリングターゲットの製造方法 |
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Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2002518593A (ja) | 1998-06-17 | 2002-06-25 | ジヨンソン マテイ エレクトロニクス,インコーポレーテツド | 微細で一様な構造とテキスチュアを有する金属製品及びその製造方法 |
JP2001020065A (ja) * | 1999-07-07 | 2001-01-23 | Hitachi Metals Ltd | スパッタリング用ターゲット及びその製造方法ならびに高融点金属粉末材料 |
US6331233B1 (en) | 2000-02-02 | 2001-12-18 | Honeywell International Inc. | Tantalum sputtering target with fine grains and uniform texture and method of manufacture |
JP2002060934A (ja) | 2000-08-24 | 2002-02-28 | Toshiba Corp | スパッタリングターゲット |
JP2002363662A (ja) * | 2001-06-01 | 2002-12-18 | Nikko Materials Co Ltd | 高純度タンタルの回収方法並びに高純度タンタルスパッタリングターゲット及び該スパッタリングターゲットにより形成された薄膜 |
WO2010134417A1 (ja) * | 2009-05-22 | 2010-11-25 | Jx日鉱日石金属株式会社 | タンタルスパッタリングターゲット |
WO2011018971A1 (ja) * | 2009-08-11 | 2011-02-17 | Jx日鉱日石金属株式会社 | タンタルスパッタリングターゲット |
WO2011018970A1 (ja) * | 2009-08-11 | 2011-02-17 | Jx日鉱日石金属株式会社 | タンタルスパッタリングターゲット |
Non-Patent Citations (2)
Title |
---|
GOOD-SUN CHOI ET AL.: "Preparation of 5N grade tantalum by electron beam melting", JOURNAL OF ALLOYS AND COMPOUNDS, vol. 469, no. 1-2, 5 February 2009 (2009-02-05), pages 298 - 303 * |
See also references of EP2604719A4 |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP2913423A1 (en) * | 2013-03-04 | 2015-09-02 | JX Nippon Mining & Metals Corporation | Tantalum sputtering target and production method therefor |
EP2913423A4 (en) * | 2013-03-04 | 2016-07-13 | Jx Nippon Mining & Metals Corp | TANTAL SPUTTER TARGET AND MANUFACTURING METHOD THEREFOR |
WO2015050041A1 (ja) * | 2013-10-01 | 2015-04-09 | Jx日鉱日石金属株式会社 | タンタルスパッタリングターゲット |
JP5969138B2 (ja) * | 2013-10-01 | 2016-08-17 | Jx金属株式会社 | タンタルスパッタリングターゲット |
Also Published As
Publication number | Publication date |
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CN103069044B (zh) | 2015-02-18 |
JPWO2012020662A1 (ja) | 2013-10-28 |
US20130098759A1 (en) | 2013-04-25 |
KR20130037215A (ko) | 2013-04-15 |
IL223879A (en) | 2015-06-30 |
TW201207124A (en) | 2012-02-16 |
EP2604719A1 (en) | 2013-06-19 |
EP2604719B1 (en) | 2020-11-11 |
TWI500778B (zh) | 2015-09-21 |
JP5389955B2 (ja) | 2014-01-15 |
SG186766A1 (en) | 2013-02-28 |
EP2604719A4 (en) | 2014-01-22 |
CN103069044A (zh) | 2013-04-24 |
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