US20050191202A1 - Method of producing target material of Mo alloy - Google Patents

Method of producing target material of Mo alloy Download PDF

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Publication number
US20050191202A1
US20050191202A1 US11/066,228 US6622805A US2005191202A1 US 20050191202 A1 US20050191202 A1 US 20050191202A1 US 6622805 A US6622805 A US 6622805A US 2005191202 A1 US2005191202 A1 US 2005191202A1
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Prior art keywords
powder
container
particle size
sintered body
average particle
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Abandoned
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US11/066,228
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English (en)
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Katsunori Iwasaki
Keisuke Inoue
Norio Uemura
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Proterial Ltd
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Hitachi Metals Ltd
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Assigned to HITACHI METALS, LTD. reassignment HITACHI METALS, LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: INOUE, KEISUKE, IWASAKI, KATSUNORI, UEMURA, NORIO
Publication of US20050191202A1 publication Critical patent/US20050191202A1/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/16—Both compacting and sintering in successive or repeated steps
    • B22F3/162—Machining, working after consolidation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/1208—Containers or coating used therefor
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps

Definitions

  • the present invention relates to a method of producing a target material of a Mo alloy by a powder sintering method.
  • a film of a refractory metal such as Mo having low electric resistance is used for a thin film electrode, thin film wiring and so on in a liquid crystal display (hereinafter referred to as LCD), which thin metal film is generally formed from a target material for sputtering.
  • LCD liquid crystal display
  • HIP hot isostatic pressing method
  • An object of the present invention is to provide a method of producing a target material of a Mo alloy, according to which method a packing density of a raw material powder in a container for pressurizing is improved, an unfavorable shape-change of a pressurized and sintered body is reduced, and a segregation of material components is decreased.
  • the present inventors examined various methods of producing the target material of the Mo alloy, and found that the above problems can be solved by controlling a particle size of the raw material powder blend which is filled into the container for pressurizing whereby attaining the present invention.
  • a method of producing a target material of a Mo alloy which comprises the steps of (a) preparing a green compact by compressing a raw material powder blend consisting of a Mo powder having an average particle size of not more than 20 ⁇ m and a transition metal powder having an average particle size of not more than 500 ⁇ m; (b) pulverizing the green compact to produce a secondary powder having an average particle size of from not less than an average particle size of the raw material powder blend to not more than 10 mm; (c) filling the secondary powder into a container for pressurizing; and (d) subjecting the secondary powder with the container for pressurizing to sintering under pressure thereby obtaining a sintered body of the target material.
  • the transition metal is any one selected from the group consisting of Ti, Zr, Hf, V, Nb, Ta, Cr and W.
  • the sintered body being enveloped in the container is subjected to hot plastic working.
  • the sintered body being enveloped with the container is subjected to hot plastic working followed by recrystallization heat treatment.
  • the raw material powder blend is preferably compressed by cold isostatic pressing. More preferably the compression is conducted under pressure of not less than 100 MPa.
  • the green compact has a relative density of not less than 50%.
  • the sintering under pressure is preferably carried out by the HIP method.
  • Preferable conditions of the HIP method are of a temperature of 1000 to 1500° C. and a pressure of not less than 100 MPa.
  • Preferably the sintered body has a relative density of not less than 98%.
  • the container filled with the secondary powder has an inner space of which maximum length is not less than 1000 mm.
  • the container filled with the secondary powder is of a metal capsule having a substantially rectangular parallelepiped form one of which face is used as an inlet opening for filling the secondary powder, the face being opposite to a bottom wall of the container forming the maximum depth, and which inner space has a maximum side length of not less than 1000 mm.
  • the hot plastic working is of plural times of plastic working under the conditions of a reduction ratio of 2 to 50% and a temperature of 500 to 1500° C.
  • the recrystallization heat treatment is carried out preferably at a temperature of 1000 to 1500° C.
  • the sintered body is sliced to obtain a plurality of tabular targets so as to maintain a maximum side length of the sintered body.
  • a packing density of a raw material powder blend in a container for pressurizing is improved, an unfavorable shape-change of a pressurized and sintered body is reduced, and a segregation of material components is decreased.
  • FIG. 1 shows schematically a longitudinal side view of a sintered body in Example 1;
  • FIG. 2 is a photograph for evaluating a Nb region segregated in a metal structure of Invention Specimen No. 2 target material in Example 1;
  • FIG. 3 is a photograph for evaluating a Nb region segregated in a metal structure of Comparative Specimen No. 9 target material in Example 1;
  • FIG. 4 is a photograph of microstructure of Specimen No. 2-1-1 in Example 3, which was taken by an optical microscope with magnification of 100;
  • FIG. 5 is a photograph of microstructure of Specimen No. 2-1-3 in Example 3, which was taken by an optical microscope with magnification of 100 .
  • a key aspect of the invention resides in the process of obtaining the green compact by compressing the raw material powder blend consisting of the Mo powder and the transition metal powder, subsequently pulverizing the green compact to produce the secondary powder having an average particle size of from not less than an average particle size of the raw material powder blend to not more than 10 mm, and filling the secondary powder into the container for pressurizing, whereby improving a packing ratio of the secondary powder in the container and decreasing a segregation of material components.
  • the present inventors found after full consideration that it is possible to improve the packing ratio of the raw material powder blend in the container by adjusting a particle size of the raw material powder blend so as to be large in some degree.
  • a particle size of the raw material powder blend so as to be large in some degree.
  • the Mo powder and the other transition metal powder are mixed, a segregation of material components is liable to occur in connection with reasons of the liability of agglomeration of the powder, the fluidity of the powder and so on.
  • the present inventors found also that it is effective for solving the problem by obtaining the green compact by compressing the raw material powder blend consisting of the Mo powder and the transition metal powder, subsequently pulverizing the green compact to produce the secondary powder, and filling the secondary powder into the container for pressurizing, whereby improving the segregation of the raw material powder blend in the container for pressurizing and also the other segregation of the material components of the sintered body in the container for pressurizing.
  • a common Mo powder has a fine particle size, which is of an average particle size of not more than 20 ⁇ m, because it is produced chemically.
  • transition metal powders of Nb, Cr, Ti and so on have a comparatively large particle size, which is of an average particle size of not more than 500 ⁇ m, because such powders are often produced by pulverizing a cast ingot.
  • the green compact is produced by compressing the fine raw material powder blend, and subsequently the green compact is subjected to pulverizing to obtain the secondary powder, having an average particle size of from not less than an average particle size of the raw material powder blend to not more than 10 mm, is produced.
  • the secondary powder is filled into a container for pressurizing and subsequently subjected to sintering under pressure, thereby obtaining the sintered body to be used for a raw material of the target material.
  • the reason why the lower limit of the average particle size of the secondary powder should be not less than the average particle size of the raw material powder blend is that it will make no sense to produce and pulverize the green compact in order to obtain a secondary powder having an average particle size less than the average particle size of the raw material powder blend.
  • the reason why the upper limit of the average particle size of the secondary powder should be not more than 10 mm is that there will be appeared clear lines of particle boundaries in the metal structure of a sintered body produced from a secondary powder having an average particle size exceeding 10 mm will have a clear boundary line, which metal structure has a kind of patterned appearance.
  • Such a sintered body implies a risk of a locally high oxygen amount because particle boundaries are in contact with the atmosphere preferentially.
  • the average particle size should be not more than 10 mm in order to make the particle boundaries not to be observed in appearance and also in order to make the particle size of the secondary powder as uniform as possible.
  • the Mo and the transition metal powders are blended, important is to produce the green compact and pulverize it, so as to have the average particle size of not more than 10 mm, in order to restrain the segregation of the transition metal powder blended with the Mo powder.
  • a size (D 50 ) of particles of which number is 50% of a total number of the particles, is referred to as the average particle (or grain) size.
  • the Mo powder to be compressed an average particle size of not more than 10 ⁇ m
  • the secondary powder obtained from the green compact by pulverizing has an average particle size of not more than 5 mm.
  • the raw material powder with a high density has a smaller particle size.
  • Mo which is a main component of the sintered body produced by the invention method
  • the raw material powder blend in the container is processed at high temperature while increasing contact areas of the particles of the raw material.
  • the average particle size of the Mo powder is not more than 10 ⁇ m.
  • the secondary powder has preferably the average particle size of not more than 5 mm is that by such a particle size, it is possible to decrease local concentration of the oxygen amount, and to enhance the dispersion of an additive element(s) in Mo alloy. More preferably, the average particle size of the secondary powder is not more than 0.5 to 3 mm.
  • the reason why the transition metal powder blended with the Mo powder has the average particle size of not more than 500 ⁇ m is that, if the average particle size exceeds this value, the segregation of component in the target material cannot be reduced.
  • the green compact preferably it is compressed so as to have a relative density of not less than 50% in order to maintain the particle size of the secondary powder to be filled into the container for pressurizing.
  • the raw material, of which primary component is Mo, is compressed preferably by a cold isostatic pressing method (herein below referred to as CIP) in which preferably a pressure not less than 100 MPa is applied to the raw material powder in order to enhance the green compact to have relative density of not less than 50%.
  • CIP cold isostatic pressing method
  • Sintering of the raw material under pressure is preferably carried out by the HIP method because it is possible to three dimensionally apply a high pressure to the raw material during sintering.
  • Desirable conditions of the HIP method are a temperature of 1000 to 1500° C. and a pressure of not less than 100 MPa. If the HIP method is carried out under a pressure of less than 100 MPa at a temperature of less than 1000° C., it is hard to produce the sintered body having a relative density of not less than 98% which is required to the target material.
  • the processing temperature of the HIP method is restricted by a material type of the container for pressurizing and an equipment.
  • an upper limit of the working temperature is approximately 1500° C. A higher temperature than 1500° C. will not be practical.
  • the invention method is suitable for producing a large size target material which requires to use the container for pressurizing which maximum length is not less than 1000 mm.
  • a way of filling the powder into the container in order to improve the packing density with utilization of a specific gravity of the powder, it is more preferable to use the container for pressurizing which has a substantially rectangular parallelepiped form one of which face is used as an inlet opening for filling the secondary powder, the face being opposite to a bottom wall of the container forming the maximum depth, and which inner space has a maximum length of not less than 1000 mm.
  • the sintered body being enveloped in the container is subjected to hot plastic working, since such working is suitable to make the sintered body to have a much larger size.
  • the hot plastic working is conducted plural times each with a reduction ratio of 2 to 50% while maintaining the sintered body at a temperature of 500 to 1500° C.
  • the temperature is lower than 500° C., a working load applied to the sintered body must be increased due to lower ductility thereof whereby arising a problem of the productivity.
  • the temperature exceeds 1500° C., there are a risk that the container is melted and a problem that crystal particles of the sintered body are coarsened.
  • the reduction ratio of the hot plastic working exceeds 50%, there arise problems that cracking and inner defects occur in the sintered body. If the reduction ratio of the hot plastic working is lower than 2%, the sintered body is hardly deformed thereby arising a waste production cost problem. Further, in the case where a high reduction working as a whole is required for the sintered body, plural times of working under the above conditions of the temperature and the reduction ratio are effective in order to avoid occurrence of cracking or other defects.
  • the sintered body is subjected to recrystallization heat treatment.
  • the work as rolled has a fiber metal structure, a degree of which structure differs every section of the work, especially at a surface portion and a central portion in the thickness direction of the work.
  • the target material should have a uniform crystal structure, since a non-uniform crystal structure of the target material adversely affect the uniformity of a film deposited by sputtering.
  • the work as rolled is subjected to homogenization treatment with utilization of the recrystallization phenomenon in order to make its crystal structure uniform.
  • the recrystallization heat treatment is preferably conducted at a temperature of 1000 to 1500° C. If the temperature is not higher than 1000° C., there is a high possibility that the fiber metal structure will remain after the heat treatment because of properties of the chemical composition with a primary component of Mo. If the temperature exceeds 1500° C., there will occur partially coarsening of crystal particles at a surface region that has previously suffered high reduction working.
  • the sintered bodies which include those merely sintered, subjected to hot plastic working and subjected to both of hot plastic working and recrystallization heat treatment, are sliced to obtain a plurality of tabular targets so as to maintain a maximum side length of the respective sintered body.
  • This method is advantageous in the point that a number of target material are produced by only one time pressurizing and sintering process in accordance with a need for a large sized target material, whereby reducing the production cost.
  • the raw powder material in the invention method contains not less than 50 atomic % Mo.
  • the Mo powder having high agglomeration property, is hard to be filled uniformly into the container for pressurizing, it is very effective to use the raw powder material in the invention method in order to obtain a target material containing not less than 50 atomic % Mo.
  • Mo powder having an average particle size of 12 ⁇ m a Mo powder having an average particle size of 12 ⁇ m, a W (tungsten) powder having an average particle size of 12 ⁇ m, a Nb powder having an average particle size of 100 ⁇ m, a Ti powder having an average particle size of 100 ⁇ m, and a Zr powder having an average particle size of 100 ⁇ m.
  • Specimen Nos. 1 to 6 target materials shown in Table 1 were produced by the following process, which are of the present invention.
  • the green compact was pulverized with utilization of a jaw crusher and a disc mill to produce a secondary powder.
  • the secondary powder was blended in a V-type blender for 10 minutes and subsequently filled into a container for pressurizing, which is made of low carbon soft steel and has an inner space dimension of a thickness of 100 mm, a width of 1000 mm and a height of 1300 mm.
  • a top lid with a deaerating port was welded to the container in order to close an inlet opening thereof.
  • the container filled with the secondary powder was subjected to a degassing process under vacuum at a temperature of 450° C. and subsequently the deaerating port was sealed. Thereafter, the secondary powder was sintered under pressure together with the container by means of a HIP machine. Operational conditions of the HIP machine were of a temperature of 1250° C., a pressure of 150 MPa and an operation time of 5 hours.
  • the thus obtained sintered body was sliced and machined to produce six tabular target materials each having a rectangular parallelepiped shape of which dimension is of a thickness of 6 mm, a width of 810 mm and a length of 950 mm.
  • a Mo powder having an average particle size of 6 ⁇ m and a Nb powder having an average particle size of 100 ⁇ m were prepared, and processed to obtain sintered bodies by the same manner as described above.
  • Each of the thus obtained sintered bodies was sliced and machined to produce six tabular target materials each having a rectangular parallelepiped shape of which dimension is of a thickness of 6 mm, a width of 810 mm and a length of 950 mm.
  • Comparative Specimen Nos. 9 and 10 target materials shown in Table 1 a Mo powder and a Nb powder were prepared. Comparative Specimen Nos. 9 and 10 target materials were produced by the following process.
  • a top lid with deaerating port was welded to the container in order to close an inlet opening thereof.
  • FIG. 1 is provided in order to describe a way how to conduct the evaluation.
  • the drawing shows schematically a longitudinal side view of a sintered body model with a x-y coordinate, in which there is a reference point 3 at a longitudinal center 2 (on the y-axis) of the bottom surface of the sintered body model 1 .
  • a left end of the sintered body model 1 is bent upwardly in the drawing so that a lowest point 4 of the left side end of the sintered body model 1 deviates from the x-axis by a distance 5 which exhibits a form variation degree.
  • FIGS. 2 and 3 show photographs for evaluating Nb regions segregated in metal structures of Invention Specimen No. 2 and Comparative Specimen No. 9, respectively.
  • Comparative Specimen No. 9 shown in FIG. 3 in which no secondary powder is produced, there exists a Nb region having a major axis of not less than 20 mm at a center of the photograph. From this, it is appreciated that a segregation of Nb occurs.
  • the Nb regions are dispersed in a Mo matrix, so that no clear segregation of Nb exists.
  • An expected size of a target material is of a width of 1500 mm and a length of 1800 mm.
  • a result of rolling of the sintered body is shown in Table 2. TABLE 2 Dimension of Objective Heating First time Second time Third time Chemical Sintered dimension temper- Total rolling rolling rolling rolling Specimen composition body in rolling ature reduction reduction reduction reduction No.
  • the target material as hot-rolled in Example 2 was subjected to a recrystallization heat treatment in vacuum at temperatures of 900° C., 1150° C. and 1300° C., respectively. After the work is heated up to a heat treatment temperature, the temperature is held for one hour, and thereafter the work is cooled.
  • Specimen Nos. 2-1-1 , 2-1-2 and 2-1-3 were taken from the three type works, respectively. Microstructures of the specimens were compared with one another with utilization an optical microscope with magnification of 100 . The observation result is shown in Table 3. With regard to the specimens subjected to a recrystallization heat treatment at temperatures of 900° C.
  • FIGS. 4 and 5 it can be seen that when a recrystallization heat treatment temperature is lower than 1000° C., there is a possibility that a fiber structure remains.

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  • Metallurgy (AREA)
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  • Manufacturing & Machinery (AREA)
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US11/066,228 2004-02-27 2005-02-25 Method of producing target material of Mo alloy Abandoned US20050191202A1 (en)

Applications Claiming Priority (2)

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JP2004055021A JP4110533B2 (ja) 2004-02-27 2004-02-27 Ｍｏ系ターゲット材の製造方法
JP2004-055021 2004-02-27

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US20070086909A1 (en) * 2005-10-14 2007-04-19 Plansee Se Method of producing a tubular target
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US20080087866A1 (en) * 2006-10-13 2008-04-17 H.C. Stark Inc. Titanium oxide-based sputtering target for transparent conductive film, method for producing such film and composition for use therein
US20100108501A1 (en) * 2007-01-12 2010-05-06 Nippon Steel Materials Co., Ltd Mo-based sputtering target plate and method for manufacturing the same
US20110117375A1 (en) * 2010-06-30 2011-05-19 H.C. Starck, Inc. Molybdenum containing targets
US20110293940A1 (en) * 2008-03-27 2011-12-01 Hitachi Metals, Ltd Coated, fine metal particles and their production method
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US20130029216A1 (en) * 2010-04-01 2013-01-31 Jungmin Kim Positive-electrode material for lithium secondary-battery, process for producing the same, positive electrode for lithium secondary battery, and lithium secondary battery
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US9334562B2 (en) 2011-05-10 2016-05-10 H.C. Starck Inc. Multi-block sputtering target and associated methods and articles
US9334565B2 (en) 2012-05-09 2016-05-10 H.C. Starck Inc. Multi-block sputtering target with interface portions and associated methods and articles
US9689067B2 (en) 2010-09-30 2017-06-27 Hitachi Metals, Ltd. Method for producing molybdenum target
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CN103182507B (zh) * 2013-03-19 2015-04-15 昆山海普电子材料有限公司 一种铬铝合金靶材的生产方法
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JP7205213B2 (ja) * 2018-03-27 2023-01-17 日立金属株式会社 ＴｉＷ合金ターゲットおよびその製造方法
JP7419886B2 (ja) * 2019-03-20 2024-01-23 株式会社プロテリアル Ｍｏ合金ターゲット材およびその製造方法
JP7419885B2 (ja) * 2019-03-20 2024-01-23 株式会社プロテリアル Ｍｏ合金ターゲット材およびその製造方法
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US8449818B2 (en) * 2010-06-30 2013-05-28 H. C. Starck, Inc. Molybdenum containing targets
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US9334565B2 (en) 2012-05-09 2016-05-10 H.C. Starck Inc. Multi-block sputtering target with interface portions and associated methods and articles
US10643827B2 (en) 2012-05-09 2020-05-05 H.C. Starck Inc. Multi-block sputtering target with interface portions and associated methods and articles
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