CN108690958A - Target cleaning method, the device for it, target manufacturing method and target and recycling ingot casting manufacturing method and recycling ingot casting - Google Patents

Target cleaning method, the device for it, target manufacturing method and target and recycling ingot casting manufacturing method and recycling ingot casting Download PDF

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Publication number
CN108690958A
CN108690958A CN201810267287.2A CN201810267287A CN108690958A CN 108690958 A CN108690958 A CN 108690958A CN 201810267287 A CN201810267287 A CN 201810267287A CN 108690958 A CN108690958 A CN 108690958A
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CN
China
Prior art keywords
target
grafting material
ingot casting
supporting member
recycling
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201810267287.2A
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Chinese (zh)
Inventor
西冈宏司
塚田洋行
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Sumitomo Chemical Co Ltd
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Sumitomo Chemical Co Ltd
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Filing date
Publication date
Priority claimed from JP2017196245A external-priority patent/JP6533265B2/en
Application filed by Sumitomo Chemical Co Ltd filed Critical Sumitomo Chemical Co Ltd
Publication of CN108690958A publication Critical patent/CN108690958A/en
Pending legal-status Critical Current

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Classifications

    • 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
    • C23C14/58—After-treatment
    • C23C14/5873—Removal of material
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B1/00—Nozzles, spray heads or other outlets, with or without auxiliary devices such as valves, heating means
    • B05B1/02—Nozzles, spray heads or other outlets, with or without auxiliary devices such as valves, heating means designed to produce a jet, spray, or other discharge of particular shape or nature, e.g. in single drops, or having an outlet of particular shape
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B13/00—Machines or plants for applying liquids or other fluent materials to surfaces of objects or other work by spraying, not covered by groups B05B1/00 - B05B11/00
    • B05B13/02—Means for supporting work; Arrangement or mounting of spray heads; Adaptation or arrangement of means for feeding work
    • B05B13/0221—Means for supporting work; Arrangement or mounting of spray heads; Adaptation or arrangement of means for feeding work characterised by the means for moving or conveying the objects or other work, e.g. conveyor belts
    • B05B13/0228—Means for supporting work; Arrangement or mounting of spray heads; Adaptation or arrangement of means for feeding work characterised by the means for moving or conveying the objects or other work, e.g. conveyor belts the movement of the objects being rotative
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B13/00—Machines or plants for applying liquids or other fluent materials to surfaces of objects or other work by spraying, not covered by groups B05B1/00 - B05B11/00
    • B05B13/02—Means for supporting work; Arrangement or mounting of spray heads; Adaptation or arrangement of means for feeding work
    • B05B13/0278—Arrangement or mounting of spray heads
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/02—Cleaning by the force of jets or sprays
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B08B3/14—Removing waste, e.g. labels, from cleaning liquid; Regenerating cleaning liquids
    • 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
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/28—Cleaning or pickling metallic material with solutions or molten salts with molten salts
    • C23G1/34—Light metals
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The present invention relates to target cleaning method, the device for it, target manufacturing method and target and recycling ingot casting manufacturing methods and recycling ingot casting.The present invention provides a kind of cleaning method of target, and the cleaning method includes following processes:From with grafting material by main target made of metal and supporting member in conjunction with and process that aforementioned target is detached in the sputtering target of formation;And by the face injection water for being attached with aforementioned grafting material to aforementioned target, the process to remove aforementioned grafting material from aforementioned target.

Description

It target cleaning method, the device for it, target manufacturing method and target and follows again Ring ingot casting manufacturing method and recycling ingot casting
Technical field
The device of cleaning method the present invention relates to the cleaning method of target, for the target, the manufacturer of target Method, target, the manufacturing method for recycling ingot casting and recycling ingot casting.
Background technology
Sputtering target (sputtering target) is typically the target that will be made of metal, alloy or ceramics with grafting material Material is formed with supporting member in conjunction with (bonding (bonding)).For target, it can be carried out after it is used Recycling, metal is melted and is cast again, is thus carried out again in the form of ingot casting (slab (slab), ingot bar (ingot)) It utilizes (recycling (recycle)).
About the recycling of sputtering target, for example, in Japanese Unexamined Patent Publication 2005-23350 bulletins, Japanese Unexamined Patent Publication 2005-23349 In number No. 2015/151498 bulletin, International Publication No. pamphlet, discloses and utilize the mechanicalnesses such as sour processing, corona treatment Removing mode removes the surface attachments of sputtering target.
Invention content
Present inventor has made intensive studies, as a result, it has been found that, for will mainly be consisted of metal with grafting material Target and supporting member in conjunction with and for the sputtering target that is formed, by after it is used by target from sputtering target point Remain the face injection water of grafting material from and then to the attachment of target and target is cleaned, thus, it is possible to easily from target Material removes accompanying grafting material.
This application involves inventions below.
[1]The cleaning method of target, the cleaning method include following processes:
From with grafting material by main target made of metal and supporting member in conjunction with and detached in the sputtering target of formation The process of aforementioned target;And
By the face injection water for being attached with aforementioned grafting material to aforementioned target, to by aforementioned grafting material from aforementioned The process that target removes.
[2]Ru [1]The cleaning method of the target, wherein the pressure of aforementioned water is 90MPa or more.
[3]Ru [1]Huo [2]The cleaning method of the target, wherein aforementioned metal is aluminium or copper.
[4]The manufacturing method of target, the manufacturing method include following processes:Implement [1]~[4]Any one of described in Cleaning method.
[5]Target, which is characterized in that it is to incite somebody to action main target made of metal and supporting member knot from grafting material The target for closing and being detached in the sputtering target of formation, also,
It can't detect the member from aforementioned grafting material and aforementioned supporting member by energy dispersion type x-ray fluorescence analysis Element.
[6]The manufacturing method of ingot casting is recycled, the manufacturing method includes following processes:By to implementing [1]~[3]In Target is cast obtained from any one of them cleaning method, to obtain including the recycling ingot casting of aforementioned metal.
[7]Recycle ingot casting, come use by oneself grafting material will main target made of metal and supporting member in conjunction with and The target of the sputtering target of formation, in the recycling ingot casting,
The total amount of element from aforementioned grafting material and aforementioned supporting member is less than 10ppm with weight basis.
[8]Ru [7]The recycling ingot casting, wherein as it is aforementioned recycling ingot casting principal component metal be aluminium or Copper.
[9]Ru [7]The recycling ingot casting, which is characterized in that the metal of the principal component as aforementioned recycling ingot casting Total amount for aluminium, foregoing impurities is less than 5ppm with weight basis.
[10]Device, described device are used for:Main target made of metal and supporting member are incited somebody to action to from grafting material In conjunction with and the face injection water for being attached with aforementioned grafting material of aforementioned target that is detached in the sputtering target that is formed, thus connect aforementioned Condensation material is removed from aforementioned target,
Described device includes:
It is used at least one nozzle head to the jet port of aforementioned target injection water at least one;
Actuator for operating former nozzle head;And
Process chamber for configuring aforementioned actuator, storage aforementioned target and handled.
[11]Ru [10]The device, described device further include:For aforementioned target to be fixed in aforementioned processing room Fixture.
[12]Ru [10]Huo [11]The device, described device further include:Tipper for making aforementioned target overturning Structure.
[13]Ru [10]~[12]Any one of described in device, described device includes drainage mechanism, the drainage mechanism Processing for the water sprayed from aforementioned jet port to be recycled to and drained, will included the grafting material removed from aforementioned target Object detaches.
Description of the drawings
[Tu1 ]To indicate the skeleton diagram of summary of the invention.
[Tu2 ]To indicate the skeleton diagram of the target of sputtering target and the combination of supporting member.
[Tu3 ]For the skeleton diagram of the combination of the target and supporting member of the sputtering target of expression another way.
[Tu4 ]For the skeleton diagram of the combination of the target and supporting member of the sputtering target of the another mode of expression.
[Tu5 ]To schematically show the approximate stereogram of the embodiment of workable device in the present invention.
[Tu6 ]To schematically show the approximate vertical view of the embodiment of workable device in the present invention.
[Tu7 ]The skeleton diagram in the section at A-A to indicate device shown in fig. 6.
[Tu8 ]The skeleton diagram in the section at B-B to indicate device shown in fig. 6.
[Tu9 ]To schematically show actuator shown in Fig. 5~8 (actuator) 103 and nozzle head (nozzle Head) the skeleton diagram of 102 relationship.
[Tu10 ]For schematically show an example as drainage mechanism UF membrane formula equipment for separating liquid from solid outline Figure.
[Tu11 ]For schematically show an example as drainage mechanism multi-stag precipitation tank skeleton diagram.
Reference sign
1 target
2 supporting members
3 grafting materials (or bonding layer)
4 solder layers
5,5 ' metal layer
10,20,30 sputtering target
100 devices
101 targets (or workpiece)
102 nozzle heads
103 actuators
103X X-axis slide blocks
103Y Y-axis sliding blocks
103Z Z axis sliding blocks
104 process chambers
105 conveying equipments
106 connecting rods
Specific implementation mode
In the present invention, for sputtering target, for example, as shown in the skeleton diagram of Fig. 1, it usually can be in the following manner It makes:To by metal molten and ingot casting obtained from casting is processed (for example, implementing calendering to obtained ingot casting, squeezing Go out equal plastic processings, then, the mechanical processings such as cut, ground), make the target with shapes such as plate or cylinder types Material, using grafting material, by the target and the backer board (backing plate) or bushing pipe as supporting member that separately make (backing tube) etc. is combined or engagement.
According to embodiment of the present invention, the sputtering target in sputtering after use can be separated into target and bearing structure Part.In turn, by separated target injection water, so as to which grafting material is removed from the target.In turn, by that will remove The target of grafting material is melted and is cast, to which ingot casting (hereinafter referred to as " recycling ingot casting ") can be obtained.By to this Recycling ingot casting is processed, so as to manufacture target.
The cleaning method of target
In the present invention, " sputtering target " is the target that will be mainly made of metal (element) with grafting material and supporting member knot Close and formed, as long as can be used for sputtering, be not particularly limited.
In the case where sputtering target is plate, as supporting member, flat backer board can be used.In addition, splashing In the case of shooting at the target as cylinder type, as supporting member, cylindric bushing pipe can be used.It herein, can be into cylinder type target Portion is inserted into cylindric bushing pipe, and the inner peripheral portion of cylinder type target can be combined with the peripheral part of bushing pipe by grafting material.
" target " can be mainly made of metal (element), such as comprising selected from by aluminium (Al), copper (Cu), chromium (Cr), iron (Fe), tantalum (Ta), titanium (Ti), zirconium (Zr), tungsten (W), molybdenum (Mo), niobium (Nb), silver-colored (Ag), cobalt (Co), ruthenium (Ru), platinum (Pt), palladium (Pd), the metal (element) in the group of golden (Au), rhodium (Rh), iridium (Ir) and nickel (Ni) composition, it includes above-mentioned metal that can be Alloy.As target, preferably Vickers hardness is usually 200 or less, preferably 100 or less, further preferably 50 below Metal or alloy.Wherein, preferably mainly by aluminium (more than purity 99.99% (4N), preferably purity 99.999% (5N) or more) or Copper (more than purity 99.99% (4N)) is constituted.Vickers hardness can pass through Vickers hardness test (JIS Z 2244:2003) confirm. The size, shape and structure of target are not particularly limited.As target, it is preferable to use the target of plate.
When target is plate, the size of the length direction of target is, for example, 500mm~4000mm, and preferably 1000mm~ 3200mm, more preferably 1200mm~2700mm.
The size of width direction (direction vertical with length direction) is, for example, 50mm~1200mm, and preferably 150mm~ 750mm, more preferably 170mm~300mm.
Thickness is, for example, 5mm~35mm, preferably 10mm~30mm, more preferably 12mm~25mm.
In the present invention, even for example, the target of large-scale flat-panel monitor, also can easily be handled.
In the case that supporting member is " backer board ", it is main comprising selected from by copper (Cu), chromium (Cr), aluminium (Al), titanium (Ti), Metal (element) in the group that tungsten (W), molybdenum (Mo), tantalum (Ta), niobium (Nb), iron (Fe), cobalt (Co) and nickel (Ni) form, Ke Yishi Include the alloy of above-mentioned metal.In the case that supporting member is " backer board ", preferably copper (oxygen-free copper), chrome copper, aluminium close Gold etc..The size, shape and structure of backer board are not particularly limited, as long as the plate of configurable target.
In the case where supporting member is " bushing pipe ", the metal of composition also with above-mentioned backer board the case where it is same.It is propping up In the case that bearing member is " bushing pipe ", preferably stainless steel (SUS), titanium, titanium alloy etc..In order to be inserted into the inside of cylinder type target And engaged, the size of bushing pipe is usually longer than cylinder type target, and the outer diameter of bushing pipe is preferably more slightly smaller than the internal diameter of cylinder type target.
" grafting material " is not particularly limited, as long as contributing to the combination of target and supporting member, can be used to form and splash The material shot at the target can (Fig. 2).Grafting material includes welding material, solder etc..
So-called " welding material " refers to the material of the metal or alloy comprising low melting point (such as 723K or less), can enumerate Including selected from being made of indium (In), tin (Sn), zinc (Zn), lead (Pb), silver-colored (Ag), copper (Cu), bismuth (Bi), cadmium (Cd) and antimony (Sb) Group in metal or its alloy material etc..More specifically, can enumerate In, In-Sn, Sn-Zn, Sn-Zn-In, In-Ag, Sn-Pb-Ag,Sn-Bi,Sn-Ag-Cu,Pb-Sn,Pb-Ag,Zn-Cd,Pb-Sn-Sb,Pb-Sn-Cd,Pb-Sn-In,Bi-Sn-Sb Deng.
As " solder ", as long as target can be combined with supporting member and fusing point less than target and supporting member gold Category or alloy, so that it may to use without particular limitation.
As grafting material, it is usually preferred to the welding materials such as the In or In alloys of low melting point, Sn or Sn alloys.
For example, welding material can by heating at the faying face with target with include in target metal (member Element) formed diffusion layer (alloy-layer) mode be combined.At the joint surface with supporting member, welding material can also be same Ground is combined in a manner of forming diffusion layer (alloy-layer) with the metal for including in supporting member (element).Therefore, by this way Welding material formed solder layer, so as to which target to be combined to (Fig. 3) with supporting member.
In general, only in the case where loading above-mentioned welding material on target or supporting member, due to target or bearing structure The influence of oxidation film that may be present, cannot get sufficient bond strength sometimes on the surface of part.Therefore, first, in order to improve Metallization (metallize) layer can be arranged in wellability of the welding material relative to their surface.
So-called " metallization " is the processing method for being generally used for that nonmetallic surface is made to realize metal membranization, the present invention In, for example, target, supporting member have oxidation film the case where when, refer to using metallization welding material, make Its with target, supporting member in conjunction with and form metal layer.
Metal layer can for example be formed by following manner:Ultrasonic wave soldering iron, the vibrational energy using ultrasonic wave are used on one side (cavitation (cavitation) effect) destroys the oxidation film of target, supporting member, makes metallization by heating on one side The metallic atom for including in the metallic atom and target that include in welding material, supporting member is together with the oxygen atom in oxidation film It is chemically bonded.In order to form metal layer, using grafting material above-mentioned.
Metal layer (5,5 ') (referring to Fig. 4) can also be combined with above-mentioned solder layer (4), be located at target (1) and solder layer (4) between, between supporting member (2) and solder layer (4), can play by target (1) and solder layer (4), supporting member (2) with The effect that solder layer (4) is securely joined with.
For the thickness of solder layer, in the case of plate, for example, 10 μm~1000 μm, preferably 50 μm~ 500 μm, in the case of cylinder type, in the range of for example, 100 μm~2000 μm, preferably 250 μm~1500 μm.
It it is usually 1 μm~100 μm in the case of plate, cylinder type, preferably for the thickness of metal layer In the range of being 10 μm~100 μm, more preferably 5 μm~50 μm.
The welding material that can be used for metallizing is, for example, comprising selected from by indium (In), tin (Sn), zinc (Zn), lead (Pb), silver (Ag), the material etc. of the metal in the group of copper (Cu), bismuth (Bi), cadmium (Cd) and antimony (Sb) composition or its alloy, more specifically, In, In-Sn, Sn-Zn, Sn-Zn-In, In-Ag, Sn-Pb-Ag, Sn-Bi, Sn-Ag-Cu, Pb-Sn, Pb-Ag, Zn- can be enumerated Cd, Pb-Sn-Sb, Pb-Sn-Cd, Pb-Sn-In, Bi-Sn-Sb etc..The appropriate selection material high with target or supporting member compatibility Material.
In the present invention, for example, as shown in the skeleton diagram of Fig. 1, after having used sputtering target in sputtering, by target from sputtering target It detaches (stripping).
The method that target is detached with supporting member is not particularly limited.For example, can on one side pair can be by above-mentioned engagement material The bonding layer (or binder course) that material is formed is heated (such as 180 DEG C~300 DEG C), bonding layer is made to be softened or melted, one side root Target is detached from sputtering target according to needing physically to destroy bonding layer.
In the case where target is plate, this side that (or engagement) is combined with supporting member of target after isolation On face (hereinafter, otherwise referred to as " faying face " or " joint surface "), usually attachment remains grafting material.Use scraper (example Such as, the scraper of organosilicon) etc. accompanying grafting material is wiped off, it is also difficult to the grafting material is removed completely.Especially It is difficult to remove the metal layer combined with target.Would generally residual thickness be several μm or so metal layer and thickness be 50 μ The solder layer of m~200 μm or so.Sometimes also attachment remains grafting material in the sputter face of target.As its reason, such as Following reasons can be enumerated:When detaching target, the grafting material of melting is attached to sputter face.As other reasons, can enumerate Following reasons:It is preserved since the target after separation being stacked on one another, thus faying face is contacted with sputter face, faying face Grafting material is attached to sputter face.
In the case where target is cylinder type, it can be used grafting material by the periphery of cylinder type target and cylindric bushing pipe Portion combines, and therefore, with plate target above-mentioned the case where is same, and grafting material is attached to the faying face (inner circumferential of the target after separation Portion), the grafting material including metal layer can not be removed completely.Sometimes also attachment remains in the sputter face of target Grafting material.It may also be mixed into as impurity sometimes from the ingredient of bushing pipe.Therefore, it for cylinder type target, can also be directed to The cleaning method is applied as the peripheral part of sputter face, inner peripheral portion.
Whether there are grafting materials about adhering on target after isolation, such as can pass through energy dispersion type X-ray Fluorescence analysis (EDXRF:Energy Dispersive X-ray Fluorescence Analysis) confirm.
It should be noted that there is also the feelings that metallic element is spread from supporting member to target (especially near joint surface) Condition.For such metallic element, can also confirm likewise by EDXRF.In addition, Wavelength dispersion type x ray can also be used Fluorescence analysis (WDXRF:Wavelength Dispersive X-ray Fluorescence Analysis), electron probe it is micro- Analyze (EPMA:Electron Probe Micro Analysis), Auger electron spectroscopy (AES:Auger Electron Spectroscopy), X-ray photoelectron spectroscopy (XPS:X-ray Photoelectron Spectroscopy), flight when Between type secondary ion mass spectrometry (TOF-SIMS:Time-of-Flight Secondary Ion Mass Spectrometry), Laser ablation inductively coupled plasma-mass spectrometry method (LA-ICP-MS:Laser Ablation Inductively Coupled Plasma Mass Spectrometry), X-ray diffraction method (XRD:X-ray Diffraction Analysis) etc. analyses side Method confirms the impurity from grafting material, supporting member, but is examined from the range of the simplicity of analysis, analyst coverage Consider, confirms preferably by EDXRF, WDXRF.
Herein, if directly manufacturing ingot casting (hereinafter, otherwise referred to as using the target after the separation for being attached with grafting material " slab " or " ingot bar ") and target is manufactured by the ingot casting, then it can be mixed into the impurity of the ingredient from accompanying grafting material. In addition, the case where spreading from supporting member to target there is also metallic element and being mixed into as impurity, such metallic element has When be also mixed into ingot casting as impurity.
In the present invention, by target after sputtering target separation, by the face at least remaining grafting material to the attachment of target Injection water cleans target, can accompanying grafting material be removed (Fig. 1) from target.It should be noted that by the cleaning, Also the metal layer combined with target can be removed.
The injection method of water is not particularly limited, preferably injection water under the following conditions.
The injection of water for example pump can be used to carry out, and preferably carry out injection water (hereinafter, otherwise referred to as " water jet with high pressure (water jet)").The pressure of injection water is, for example, 90MPa or more, preferably 90MPa~350MPa, more preferably 100MPa ~300MPa, further preferably 150MPa~280MPa, particularly preferably 180MPa~250MPa.By improving injection pressure, Grafting material, especially metal layer can be removed, sufficient cleaning performance can be obtained.By reducing injection to a certain extent Pressure, thus prevents beyond metal layer and reams target itself deeper.If reaming deeper, such as 1.5mm or more Target itself then there is a possibility that yield rate is deteriorated or cost of equipment improves.
It is preferable to use the nozzle heads of rotary (or can rotate) with multiple jet ports (or nozzle) to come for the injection of water It carries out.The shape of nozzle head is not particularly limited, the face of this side towards target of nozzle head (or this side of setting nozzle Face) shape be, for example, the polygons such as triangle, quadrangle, circle, ellipse, due to making its rotation carry out injection water, thus The regular polygons such as preferably circular and square, more preferably circular.It is handled on the joint surface to plate target In the case of, it is preferable to use can be jet port can be installed in a manner of the direction injection water substantially parallel with the rotary shaft of nozzle head Nozzle head.In the case where the joint surface (inner peripheral portion) to cylinder type target is handled, it is preferable to use can with can along with nozzle The mode of the rotary shaft generally perpendicular direction injection water of head installs the nozzle head of jet port.
The number (or number of nozzle) for the jet port being arranged in 1 nozzle head is not particularly limited, for example, 1 with On, preferably 1~15, more preferably 3~10.Number of nozzle is suitably determined according to the size of nozzle head. By increasing number of nozzle, it can prevent grafting material etc. from not reamed and being remained, or prevent processing time elongated.Number of nozzle When more, total spray volume increases, therefore, it is necessary to larger and expensive pump, the case where there are cost of equipment raisings.In nozzle head In when being provided with multiple jet ports, jet port can be configured to the same path position in nozzle head, can also be configured in reducing position.Separately Outside, can also be the combination of same diameter configuration, reducing configuration.
The size (nozzle diameter) of jet port is, for example, 0.1mm or more, preferably 0.15mm~0.50mm, more preferably 0.2mm~0.35mm.The identical jet port of diameter nozzle head can be installed on, also the different jet port of diameter peace can be combined Loaded on nozzle head.
The spray volume (or water) of water changes according to the pressure of the water of injection, the difference of the size of jet port, water Spray volume it is bigger, then cleaning performance is better.Total spray volume of the water sprayed from all jet ports of 1 nozzle head is, for example, 2.0L/min or more, preferably 2.0L/min~42L/min, more preferably 5.0L/min~30L/min, further preferably 5.0L/min~20L/min.
The injection of water preferably by being maintained a certain distance on one side the process face relative to target, while with certain speed In the horizontal direction by band-like (threadiness) carry out it is mobile in a manner of carry out.For the injection of water, can same position repeatedly Carry out for several times, preferably 1 time~3 times.Alternatively, when the case where the processing width of 1 water injection is less than target width, it can be with (overlapping (overlap)), which is locally repeated, with threadiness carrys out injection water.
The movement speed of nozzle head is, for example, 100mm/min or more, preferably 500mm/min~7000mm/min, more excellent It is selected as 900mm/min~5000mm/min.By increasing movement speed, processing time can be shortened.It, can by reducing movement speed Obtain sufficient cleaning performance.
The rotary speed of nozzle head is, for example, 500min-1More than, preferably 500min-1~4000min-1, more preferably 900min-1~2500min-1.By increasing rotary speed, according to the number of nozzle, can wash by water to target entire surface to prevent Grafting material etc. is not reamed and is remained.If reducing rotary speed, impact when colliding target becomes larger, therefore, can be filled The cleaning performance divided.
The distance between nozzle head and target (or nozzle distance) are, for example, 10mm or more, preferably 15mm~100mm, more Preferably 20mm~70mm.By increasing distance to a certain extent, the influence for colliding the water to rebound after target can be prevented, as a result, Sufficient cleaning performance can be obtained.By reducing distance to a certain extent, to make impact when collision target become larger, therefore, Sufficient cleaning performance can be obtained.
It for the water of injection, is not particularly limited, as long as the impurity not comprising particle shape as meeting plug nozzle Or dust etc., the use of such as tap water, pure water can be enumerated.In addition, filter can be arranged between pump and nozzle, pass through The filter and injection water.
The injection direction of water is not particularly limited, as long as the angle of water collision target can be made, it can be relative to target Material is vertical, can also be tilted relative to target.For example, angle (central shaft of jet port and the hanging down perpendicular to target of jet port Angle formed by line) be 0 °~60 °, preferably 0 °~45 °, more preferably 5 °~45 °, further preferably 5 °~30 °, more into one Preferably 8 °~30 °, particularly preferably 10 °~25 ° of step.From direction injection water inclined relative to target, by It is rotated in nozzle head, thus compared with vertical the case where spraying, processing width becomes larger.Having collided the water to target will not be detained In process face, but outside is escaped into, therefore also it can be expected that the raising of cleaning performance.If from nozzle head obliquely injection water, Also it can implement the cleaning of side in the state of so that nozzle head is located above target.
By the way that the injection direction of water to be set in above-mentioned range, impact when can prevent from colliding target is reduced, and can be obtained To sufficient cleaning performance.In addition, the processing of the processing on joint surface, the processing of sputter face, side about target, need not weigh New setting target or the position for changing nozzle head, therefore processing time can be shortened.Multiple jet ports are provided in nozzle head When, the angle of each nozzle can be the same or different.For the angle of each jet port, as expected processing is wide It spends and to be not in by being suitably determined in a manner of remaining part not in contact with not reamed caused by water.
For former nozzle head, in order to shorten the processing time of every 1 target, multiple nozzle heads can be made to carry out simultaneously Scanning.
Above to having used revolving nozzle head the case where, is illustrated, but the case where target can be made to rotate Under or using can with it is linear come injection water flat fire type nozzle head in the case of, also can be high using fixed nozzle head Effect ground cleaning target.
If being sufficiently carried out the behaviour for removing grafting material, metal layer from the joint surface of used target by cleaning Make, then the surface of target itself can also be reamed.At this point, the surface of target itself can be reamed such as 5 μm in a thickness direction Above, preferably 10 μm or more 1000 μm or less, preferably 20 μm or more 750 μm or less, more preferable 50 μm or more 500 μm hereinafter, should Surface after cleaning can form pear skin shape (Japanese:Pears ground shape).Also it can be formed corresponding with the action of nozzle head when cleaning all The cutter trade (squamous, helical form etc.) of phase property.In the case where forming pear skin shape, the wavelength 300nm on the surface after cleaning~ Normal reflection rate at 1500nm is usually 1.0% hereinafter, in order to confirm that the impurity from grafting material and supporting member is abundant It removes, preferably 0.7% or less.
If in addition, with the change rate (cleaning of the normal reflection rate at the wavelength of each incident light in wavelength 300nm~1500nm The normal reflection rate on the surface before the normal reflection rate/cleaning on surface afterwards) become usual 0.025 or more 0.85 or less, preferably 0.05 Above 0.75 or less, more preferable 0.08 or more 0.60 or less, further preferred 0.10 or more 0.40 mode below is cleaned Processing, then can not only confirm that the impurity from grafting material and supporting member is fully removed, but also can prevent beyond necessarily Excessively ream target.
Arithmetic average roughness Ra at the joint surface of target after cleaning is 5 μm or more, and engagement material is come from order to confirm Material and the impurity of supporting member are fully removed, preferably 10 μm or more, more preferably 15 μm or more.Preferably, before with cleaning Change rate (the calculation on the surface before the arithmetic average roughness Ra/ cleanings on the surface after cleaning of arithmetic average roughness Ra afterwards Art average roughness Ra) become 4 or more 80 or less, preferably 5 or more 50 or less, it is more preferable 7.5 or more 20 or less, further preferably 10 or more 15 modes below start the cleaning processing.
Arithmetic average roughness Ra at the joint surface of target after cleaning be usually 100 μm hereinafter, preferably 50 μm with Under.When arithmetic average roughness Ra is excessive, it may occur however that following situations:The foreign matters such as dust or the grains of sand are easy attachment, alternatively, oxidation The thickness of film thickens, and the impurity recycled in ingot casting increases.
Cleaning method through the invention can decrease below the amount from grafting material and the element of supporting member The Monitoring lower-cut of EDXRF is (in general, Monitoring lower-cut is different according to the difference of element, for example, the inspection of the impurity from grafting material It is 0.01 weight % or so to survey lower limit, is 0.01 weight % for example, for indium) value.That is, it is a feature of the present invention that In target after cleaning, substantially can't detect the element from grafting material and supporting member, (or the target after cleaning is real The element from grafting material and supporting member is not included in matter).
In the present invention, so-called " substantially can't detect the element from grafting material and supporting member " (or " substantially not Including the element from grafting material and supporting member "), as described above, referring to:Element from grafting material and supporting member Amount decrease below the Monitoring lower-cut of EDXRF and the degree that can not be detected by EDXRF.Herein, so-called from engagement material " impurity " of material or supporting member only indicates to constitute grafting material or the essential element of supporting member.It is so-called " to come from grafting material With the element of supporting member ", refer to constituting grafting material or the essential element of supporting member.Relative to grafting material or bearing structure For 100 mass parts of part, the element is with the amount more than usual 0.1 mass parts, preferably 0.5 mass parts, more than more preferable 1 mass parts By comprising.
For the present invention cleaning method for, with as the machining carried out using milling cutter in the position of certain altitude The method set as being processed into plane is different, is only efficiently to cut on the surface for the target (or workpiece) that the water of injection is collided The method gone.Therefore, for the cleaning method of the present invention, even if target can be with high finished product rate if there is concave-convex or deformation It is handled, is applicable not only to start the cleaning processing the joint surface of target, but also suitable for being formed by sputtering Has the sputter face of irregular target, the joint surface inside cylinder target starts the cleaning processing.
In addition, for the cleaning method of the present invention, due to that can not consider the highly setting workpiece of process face, so Can in the case that setting, cleaning do not need it is time-consuming easily carry out, therefore, the previous side with plasma, cutting etc. Method is compared, and is had the advantages that more.
Device
The invention further relates to the devices that can be used in above-mentioned cleaning method.Specifically, it is related to being used for following purposes Device (hereinafter, being also referred to as " cleaning device " sometimes):By being stated at least up from will be mainly by metal with grafting material The target of composition and supporting member in conjunction with and being attached in the target (or used target) that is detached in the sputtering target that is formed The face injection water of grafting material, to remove grafting material from target.
Cleaning device at least may include composition (a)~(c) below.
(a) at least one nozzle head to the jet port of target injection water is used for at least one
(b) it is used to operate or the actuator of moving nozzle head
(c) it is used to configure actuator, storage target and the process chamber handled
For example, as shown in figures 5-8, device 100 includes at least:
It can be at least one of the jet port (not shown) of 101 injection water of used target (or workpiece) at least one Nozzle head 102;
The actuator of (or mobile) nozzle head 102 can be operated, the actuator preferably has X-axis slide block (slider) 103X, Y-axis sliding block 103Y and Z axis sliding block 103Z, the structure in a manner of any direction of the nozzle head 102 in XYZ axis can be made to move At actuator 103;And
It can configure actuator and target 101 can be stored and handled the process chamber 104 of (or cleaning).
In the mode of diagram, target 101 is described with plate, but workable target 101 is not limited in device 100 It is plate.
Nozzle head
For nozzle head, as long as the nozzle head of the jet port (or nozzle) at least one energy injection water, so that it may To use without particular limitation.In addition, the number for the nozzle head used is also not particularly limited.Using multiple nozzles In the case of head, preferably interval is appropriately spaced from such a way that the water sprayed from nozzle does not interfere and configured.
In addition, in addition the device of the invention can also have:Nozzle for being cleaned to the side injection water of workpiece Head (or side spray mouth).For in order to the side (faces X-Z and/or the faces Y-Z) to workpiece handled and the nozzle head that uses Number and allocation position are not particularly limited.
As nozzle head, the spray being described in detail in above-mentioned " cleaning method of target " can be suitably used without restriction Mouth.
Can also have the rotary unit for making nozzle head rotate.
Actuator
As actuator, operated using the driving force based on electricity, oil pressure, air pressure etc. can be utilized or moving nozzle head Device.It is preferable to use can arbitrarily appropriate moving nozzle head actuates along at least one of X-axis, Y-axis and Z axis direction Device, more preferably use can distinguish the actuator of arbitrarily appropriate moving nozzle head along all directions in X-axis, Y-axis and Z axis.
More specifically, for all direction moving nozzle heads in X-axis, Y-axis and Z axis, for example, such as Fig. 5 can be used Such 3 axis with X-axis slide block 103X, Y-axis sliding block 103Y and Z axis sliding block 103Z shown in~9 (especially Fig. 9) are combined Actuator 103.
For nozzle head 102, for example, with can it is equal via connecting rod (rod) 106 as needed and directly or indirectly with The mode of Z axis sliding block 103Z connections is constituted, using Z axis sliding block 103Z make nozzle head 102 along Z-direction (upper and lower directions or Close to the direction of the processed surface of target 101 or the direction of the processed surface of separate target 101) mobile (Fig. 9).In another way In, Z axis sliding block 103Z can be constituted through its inside in a manner of by connecting rod 106.
Z axis sliding block 103Z is available can be constituted physically or in a manner of mechanical system is connect with Y-axis sliding block 103Y Y-axis sliding block 103Y make nozzle head 102 together with sliding block 103Z along Y direction (with the direction of travel of target 101 or the dress of diagram Set the vertical direction of length direction of 100 or target 101) mobile (Fig. 9).
Y-axis sliding block 103Y is available can be constituted physically or in a manner of mechanical system is connect with X-axis slide block 103X X-axis slide block 103X makes nozzle head 102 together with sliding block 103Y and 103Z along the X-direction (direction of travel or diagram of target 101 Device 100 or target 101 length direction) mobile (Fig. 9).In addition, Y-axis sliding block 103Y's connect with X-axis slide block 103X The end of the opposite side of end can with can be relative to the support guide rod (support that X-axis slide block 103X is parallelly configured Guide) (or guide rail) engages.
By using the actuator 103 (Fig. 9) including such sliding block 103X, 103Y and 103Z, 102 edge of nozzle head can be made It suitably moves in these three directions of X-axis, Y-axis and Z axis.
For sliding block 103X, 103Y and 103Z, as long as the driving force based on electricity, oil pressure, air pressure etc. can be utilized It slidably moves, then its type of drive, connection type is not particularly limited each other.
The movement of nozzle head based on actuator and the injection of water can be controlled by electronic program.In this case, may be used Suitably each sliding block to be connected with cable etc..For the injection of the movement speed of nozzle head and water, preferably according to above-mentioned " cleaning method of target " defined in as controlled.
Actuator can be water proofing property, by for water proofing property, thus preventing:Due to injection water or collide target and The droplet contact actuator of the water of generation and the unfavorable condition caused by the rust or oil starvation that generate.In addition, will be actuated with cable When each sliding block connection of device, for cable, preferably also water proofing property.
Embodiment that can be as shown is such, as needed, also can be further from nozzle head to vertical lower injection water Configuration can change the mechanism of the angle of nozzle head.It in this case, can be by electronic program, together to the angle of nozzle head It is controlled.In addition, mechanism in this way, can more efficiently clean the target of cylinder type.
As actuator, for example, the industrial robot that can be used 3 axis of IAI CORPORATION combined.
It should be noted that for workable actuator in the apparatus of the present, above-mentioned actuate should not necessarily be limited by Device and explain.
Process chamber
The main purpose of process chamber is:Above-mentioned actuator and nozzle head can be configured simultaneously, target is stored, according to above-mentioned " cleaning method of target " target is handled.
By being handled target in process chamber, can prevent:The water sprayed from nozzle head collides target and generates The droplet of water, the solids treatment object (or dust) comprising the grafting material removed from target disperse to surrounding and pollute environment.
For example, as shown in figures 5-8, process chamber 104 has the main body of rectangle, and upper part is opened, can configure rush The mode of dynamic device (the specifically actuator 103 shown in Fig. 9 for including sliding block 103X, 103Y, 103Z) is constituted.
The size of process chamber 104 is not particularly limited, the target of large-scale sputtering target can preferably be handled.
When embodiment as shown conveys target 101 along the length direction of target 101 like that, the X-axis of process chamber 104 The ratio between the size in direction and the size of Y direction (X/Y) are, for example, 3/16~10/1, preferably 1/2~10/3, more preferably 6/ 7~7/3.
The ratio between the size of X-direction and the size of Z-direction (X/Z) they are, for example, 1/3~10/1, and preferably 1/2~4/1, More preferably 5/6~35/12.
The ratio between the size of Y direction and the size of Z-direction (Y/Z) they are, for example, 1/5~8/1, and preferably 3/5~2/1, more Preferably 5/6~35/24.
In these cases, the size of X-direction is, for example, 750mm~5000mm, preferably 1000mm~4000mm, more Preferably 1500mm~3500mm.
The size of Y direction is, for example, 500mm~4000mm, preferably 1200mm~2000mm, more preferably 1500mm ~1750mm.
The size of Z-direction specifically be, for example, 500mm~2500mm, preferably 1000mm~2000mm, more preferably For 1200mm~1750mm.
In the illustrated embodiment, by using conveying equipments 105 such as described further below ribbon conveyer, rollers, So as to convey target 101 along the length direction of target 101, target is handled in the inside of process chamber 104, but also can edge The width direction (direction vertical with length direction) (such as along Y-axis) of target 101 conveys target 101, in process chamber 104 Portion handles target 101.
In the case where the width direction (direction vertical with length direction) along target 101 conveys target 101, process chamber The ratio between the size of 104 X-direction and the size of Y direction (X/Y) they are, for example, 3/16~10/1, and preferably 1/2~10/3, more Preferably 6/7~7/3.
The ratio between the size of X-direction and the size of Z-direction (X/Z) they are, for example, 1/3~10/1, and preferably 1/2~4/1, More preferably 5/6~35/12.
The ratio between the size of Y direction and the size of Z-direction (Y/Z) they are, for example, 1/5~8/1, and preferably 3/5~2/1, more Preferably 5/6~35/24.
In these cases, the size of X-direction is, for example, 750mm~5000mm, preferably 1000mm~4000mm, more Preferably 1500mm~3500mm.
The size of Y direction is, for example, 500mm~4000mm, preferably 1200mm~2000mm, more preferably 1500mm ~1750mm.
The size of Z-direction is, for example, 500mm~2500mm, preferably 1000mm~2000mm, more preferably 1200mm ~1800mm.
Using conveying equipment 105, process chamber 104 can have for making conveying equipment 105 and target 101 By a pair of openings portion (input port, delivery outlet).The size of opening portion is not particularly limited, as long as target 101 can be made By.
Embodiment as shown is such, when conveying target 101 along the length direction of target 101, the Y direction of opening portion Size be, for example, 100mm or more, preferably 150mm~1500mm, more preferably 200mm~1000mm, even more preferably Size for 250mm~500mm, Z-direction is, for example, 10mm or more, and preferably 12mm~300mm, more preferably 20mm~ 200mm is even more preferably 45mm~150mm.
In the case where the width direction (direction vertical with length direction) along target 101 conveys target 101, opening portion The size of X-direction be, for example, 500mm or more, preferably 750mm~4000mm, more preferably 1000mm~3500mm, into One step is more preferably 1500mm~3000mm, and the size of Z-direction is, for example, 10mm or more, and preferably 12mm~300mm is more excellent It is selected as 20mm~200mm, is even more preferably 45mm~150mm.
In the above-described embodiment, the device that can convey target 101 is illustrated, but the cleaning device of the present invention It can be not provided with conveying equipment 105.
In embodiment shown in Fig. 5, in order to fully observe process chamber 104 inside situation, in its side (faces X-Z) also the mode with opening portion indicates that such opening portion may exist, and can not also exist.As presence In the case of opening portion, can the door (for example, the door split around) of open and close type be set in the opening portion, to prevent water Droplet, dust disperse.By door as setting, to make the maintenance of the inside of process chamber 104 become easy thus excellent Choosing.
Bottom in the inside of process chamber 104 can have and be sprayed from nozzle head and to target 101 for temporarily storing Water (containing the solids treatment object (or dust) comprising the grafting material removed from target) after being cleaned is (hereinafter referred to as " processing water ") storage pool (pool) (not shown).
In the inside of process chamber 104, there can be the outlet (not shown) for processing water to be discharged.Outlet can by with It sets in the bottom surface of process chamber 104, but due to being also likely to be present processed material accumulation and the case where block outlet, thus can also be with Bottom surface separates the interval of such as 1mm~50mm, preferably 10mm~25mm and is configured in side.For outlet, to it Shape, size and structure are not particularly limited, as long as can be by processing water discharge.
It is used to rinse the internal face for being attached to process chamber 104 in addition, can optionally have in the inside of process chamber 104 The spraying mechanism of processed material.
For workable process chamber in the device of the invention, it should not necessarily be limited by above-mentioned process chamber and explain.
Other structures
Device may also include other structures other than above-mentioned structure.
Fixture
The device of the invention may also include for target to be fixed on the indoor fixture of processing.By fixing target with fixture Material, so as to by during cleaning treatment target do not move in a manner of target is fixed.For configuring fixture in process chamber Position is not particularly limited.It is preferred that being fixed from the both sides of target by the side of target.By being fixed in the manner described above, from And can be in the case where the processed surface of target is not covered by fixture, to processed surface entire surface injection water.
The case where target deforms, when bending to the case where arch, if from the upside injection water of target, also deposit The case where the effect of target vibration, cleaning treatment declines, but by as described above being fixed the side of target with fixture, from And it can inhibit the vibration of target.
In the few situation of the warpage of target or in the case where the downside of target has pedestal, in order to from the vertical of target Top injection water is only fixed in such a way that target will not be moved from predetermined specified position.
By the way that target is fixed on predetermined specified position (location determination of target) with fixture, to also available Following such advantages:When carrying out the operation of nozzle head, zero adjustment (process range specified) need not be carried out.
There is no limit, it is preferable to use can be in the manner described above from the both sides of target by target for shape and size for fixture etc. The fixed fixture in side of material.The side fixture of such as IMAO CORPORATION, Tsudakoma Corp can be used (side clamp) etc..The number of fixture, the position of configuration fixture are not particularly limited, are suitably determined i.e. according to target It can.
The mechanism of fixture can be automatic, or manually, excellent in order to make the simple operation of fixed large-scale target It is selected as when specified position is provided with target, from self-action as the side of the sandwich target of target.In addition, in fixture In the case of for hand, from the aspect of operability, it is preferred that be arranged in 104 side of process chamber (faces X-Z) and be open The door of portion, preferably open and close type.
Conveying mechanism
The device of the invention may include the conveying mechanism (example that can be inputted target into process chamber, export target from process chamber Conveying equipment 105 as shown in figures 5-8).
As conveying mechanism, as long as the mechanism of target can be conveyed, so that it may to use without particular limitation, example can be enumerated Such as ribbon conveyer, roller conveyor, crawler belt conveyer, shuttle (shuttle) conveying, supporting plate conveying, vacuum cup conveying, Robotic arm conveying etc..
Speed for being conveyed target using conveying mechanism is not particularly limited, for example, 15m/ minutes~60m/ minutes, Preferably 20m/ minutes~50m/ minutes, more preferably 25m/ minutes~40m/ minutes.
Conveying mechanism can be formed with can after exporting target from process chamber, the mode that is inputted again into process chamber it is continuous Circuit (loop).
For conveying mechanism, it can be used according to input, output is used, handles the purpose of indoor, circuit and arbitrary Ground Split.
In addition, for conveying mechanism, the feed mechanism of target can be set in the entrance side of process chamber, can located Manage the switching mechanism of the outlet side setting target of room.
The feed mechanism of target
The device of the invention can include the confession of target in a manner of it can be properly supplied target to above-mentioned conveying mechanism To mechanism.The feed mechanism of target is not particularly limited, as long as target can be properly supplied.In addition, the supply machine of target Structure may include the case for storing multiple targets, can be the feed mechanism that can be properly supplied target from the case as needed. As the feed mechanism of target, commercially available automatic supplier can be used.
The switching mechanism of target
The device of the invention also may include:For make target overturn switching mechanism, preferably can with target is fixed (such as Be fixed with fixture etc.) state make the mechanism of target overturning.By comprising such switching mechanism, so as to make target The processed surface of material is arbitrarily overturn.The size of switching mechanism is not particularly limited.
Commercially available automatic turning device can be used, for example, Adpec., the automatic turning device etc. of Ltd. can be used.
Drainage mechanism
Due to the processing water after cleaning target contain include the grafting material removed from target solids treatment object (or powder Dirt) etc., therefore, the device of the invention may include that drainage mechanism, the drainage mechanism preferably can be from the processing water as needed In recycle-water and drained, by the solids treatments object such as grafting material detach.
As drainage mechanism, as long as the mechanism that can detach solid with liquid, so that it may to use without particular limitation. As needed, equipment for separating liquid from solid etc. well-known in the field can usually be suitably used.
Drainage mechanism is preferably connect with the outlet for the inside that may be disposed at process chamber.
For example, using the equipment for separating liquid from solid for the UF membrane formula for being generally used for water process.For consolidating for UF membrane formula For liquid separating apparatus, the use of at least one includes the multiple bellows (film cartridge) for the film that can be separated by solid-liquid separation, lead to The collector pipe being connect with the bellows is crossed, water is filtered with pump, thus the water of recycling can be expelled to external (Figure 10).This When, processed material can be deposited in the bottom of slot, therefore, also can separately be recycled and be recycled.
As drainage mechanism, using the precipitation tank that can be detached solid with liquid by precipitation.Such as it can enumerate logical It often can be used for funnel (hopper) type precipitation tank, round precipitation tank, the cross-flow type with centre-drive scratch device of water process Precipitation tank etc..By using such precipitation tank, the solids treatment object for including the grafting material removed from target can be separately recycled.
Alternatively, the precipitation tank of multi-stag as shown in Figure 11 can be utilized to detach solid with liquid.Multi-stag is sunk Shallow lake slot has multiple precipitation tanks, can be successively from the high precipitation tank of water level to the low precipitation tank of water level, downward from the top of precipitation tank The precipitation tank draining of grade.Processed material is deposited in the bottom of each precipitation tank, can separately be recycled object and be recycled.
The capacity of series and each precipitation tank for precipitation tank is not particularly limited.In addition, from precipitation tank to next precipitation Pump can be used to carry out for the draining of slot.
Side spray mouth
The device of the invention can include at least one in process chamber at least 1 for the side injection water to target The side spray mouth of a nozzle.About side spray mouth, can be said as described above using in above-mentioned " cleaning method of target " Bright nozzle head.Side spray mouth can be fixed, or movable.In the case that side spray mouth is movable, preferably So that side spray mouth is moved along X-axis or Y-axis and uses.
The position and its number that configure side spray mouth are not particularly limited.
By as needed by use such side spray mouth, so as to implement not only for target interarea but also Include the three-dimensional cleaning treatment of its side.
Pump
The device of the invention may include the pump that water can be supplied to above-mentioned nozzle head and/or side spray mouth.As pump, such as It may be used at the pump illustrated in above-mentioned " cleaning method of target ".
Pump can be by the pipeline that can be fluidly connected, the preferably pipeline of resistance to pressure and nozzle head and/or side spray mouth Connection.Such pipeline can arbitrary disposition, for example, can pass through along connecting rod shown in Fig. 5~8 106 or from the inside of connecting rod 106 And it is configured.It is described to pump the inside for being configured in process chamber, outside, it is preferably arranged at the outside of process chamber.In addition, The number of pump for using is not particularly limited, and multiple pumps can be used.
Control device
Control device can be used to suitably control for above-mentioned structure.As control device, can enumerate for example with The equipment of CPU, ROM, RAM etc..Above-mentioned structure can be arbitrarily selected, is electrically connected, as needed, using electronic program, Above structure is controlled by the control device.
Drier
The device of the invention can include for will adhere on used target after cleaning inside and outside process chamber The drier that water rapidly removes.By removing water, to be carried out as raw material using the used target after cleaning When fusing, casting, a problem that foreign matter occurred due to the water adhered on raw material being prevented to be mixed into.
As drier, such as can be used:Based on blowing dry air or nitrogen etc. to the used target after cleaning Gas, the drier that the water adhered on target is blown to winged air-supply;Based on the dry of the heating using hot wind, heating plate progress Dry mechanism.Process chamber 104 have for make conveying equipment 105 and target 101 by opening portion (delivery outlet) when, preferably in advance The drier based on air-supply is arranged in adjacency section inside or outside opening portion.
[The You Xuanshishifangshi &#93 of cleaning device;
In a preferred embodiment, device includes:
Nozzle head,
Actuator,
Process chamber, and
In the group being made of fixture, side spray mouth, switching mechanism, drainage mechanism, drier and conveying mechanism At least one inscape.
For the device of the invention, it should not necessarily be limited by including the device of above structure and explain.
Recycle the manufacturing method of ingot casting
Such as it as shown in Figure 1, is obtained by will utilize the manufacturing method of the process of the cleaning method including implementing the present invention To target melt and cast, recycling ingot casting can be manufactured.
As the method for manufacture recycling ingot casting, the target cleaned according to the present invention can be used, by melting, casting The process made manufactures.Fusing, casting can be carried out by known step.It recycles in ingot casting, as melting method, uses electric furnace Or combustion furnace in an atmosphere or in vacuum melts it, and as casting method, continuous casting process, semi-continuous casting can be used Method, mold castings, microcast process, heat top casting, gravitation casting method etc..In addition, can be real between fusing, casting process Apply degassing process, field trash removing processing.
For recycling the manufacturing condition (temperature etc.) of ingot casting, according to the metal (element) for including mainly in target It is suitably determined.
In target as principal component and by comprising metal be aluminium when, (for example, 0.03Torr) or air under vacuum Under, in 670~1200 DEG C, preferably 750~850 DEG C, the target fusing after cleaning is made in the crucible of carbon or aluminium oxide etc., according to It needs to be stirred in an atmosphere, after removing removing dross, is cooled down in an atmosphere, recycling ingot casting can be manufactured as a result,.
In target as principal component and by comprising metal be copper when, (for example, 0.03Torr) or air under vacuum Under, in 1100~1500 DEG C, preferably 1150~1200 DEG C, the target fusing after cleaning is made in the crucible of carbon or aluminium oxide etc., It is stirred in an atmosphere as needed, after removing removing dross, is cooled down in an atmosphere, recycling ingot casting can be manufactured as a result,.
It for recycling the manufacture of ingot casting, can manufacture, can also merge previous merely with the target after cleaning Raw metal and cleaning after the mixture of target use.
When mixing the target after raw metal and cleaning, the mixed proportion of the target after cleaning is usually 20 weight % More than, in order to inhibit the ratio of the expense of raw materials in manufacturing cost, preferably 50 weight % or more.
Recycle ingot casting
The recycling ingot casting of the present invention will main target made of metal and supporting member knot come grafting material of using by oneself Close and formed sputtering target target recycling ingot casting, as described above, which is characterized in that substantially do not include from engagement material The element of material and supporting member, can have the composition substantially identical with original (not used) target.Therefore, can by it is above-mentioned again Recycle target of the ingot casting manufacture with the composition substantially identical with original target.
So-called herein " having the composition substantially identical with original target ", refers to that main metal (element) is identical, can Including the impurity with the amount that the impurity contained by script in original target is equal extent.
In above-mentioned recycling ingot casting, the total amount of the impurity from grafting material and supporting member is usually low with weight basis In 10ppm, preferably 0.1ppm~8ppm, more preferably 5ppm or less (or being less than 5ppm), is even more preferably 0.1ppm ~5ppm is even more preferably 0.1ppm~2ppm.In above-mentioned recycling ingot casting, the total amount of all impurity is such as less than 50ppm, preferably 0.1ppm~20ppm, more preferably 0.1ppm~10ppm, further preferably 5ppm or less (or be less than 5ppm), even more preferably in the range of 0.1ppm~5ppm.It should be noted that the impurity for including in original target And its amount can depend in the target as principal component and by comprising metal type and original target manufacturing method.
Recycling ingot casting can also be used for the purposes other than target, also can be used as aluminium electrolutic capacitor, hard disk substrate, corrosion-resistant Property material, high-purity alpha-alumina etc. require the raw material of the product of high-purity to use.
In target as principal component and by comprising metal be aluminium when, recycle ingot casting in include come from grafting material Total amount with the element of supporting member is with weight basis such as less than 10ppm, preferably 0.1ppm~8ppm, more preferably 5ppm or less (or being less than 5ppm), further preferably 0.1ppm~5ppm is even more preferably 0.1ppm~2ppm.Although Depending on purposes, but for example for the aluminum target of flat-panel monitor, even if containing usual 50ppm or less, preferably The impurity of 0.1ppm~20ppm, more preferable 0.1ppm~10ppm, even more preferably 5ppm or less (or being less than 5ppm), also not Sputtering can especially be interfered.
In target as principal component and by comprising metal be copper when, recycle ingot casting in include come from grafting material 10ppm, preferably 0.05ppm~9ppm are usually less than with weight basis with the total amount of the element of supporting member, more preferably 0.05ppm~8ppm.Although depending on purposes, such as the anaerobic of flat-panel monitor target made of copper, it is known that Wherein can include the impurity of usual 100ppm or less, preferably 0.1ppm~75ppm, more preferable 0.1ppm~50ppm, if impurity Amount is above-mentioned degree, then will not especially interfere sputtering.
The amount for the impurity for including in recycling ingot casting is denier, and therefore, the amount of such impurity can utilize glow discharge Mass spectrography (Glow Discharge Mass Spectrometry (GDMS)) measures.The lower limit of quantitation of GDMS is according to the master of target Element and different as the detection element of object, for example, as target principal component and by comprising metal for aluminium when, usually It is 0.01ppm for example, for indium for 0.001ppm~0.1ppm.
As described above, through the invention, can easily clean used target, the target after cleaning does not include substantially Element from grafting material and supporting member.Therefore, pass through the above-mentioned target to being handled using the cleaning method (or recycling) is recycled, the substantially recycling not comprising the element from grafting material and supporting member can be obtained and cast Ingot.That is, through the invention, the target with the composition substantially identical with original target can easily be made to regenerate.
It through the invention, can be by grafting material (welding material, pricker existing for the surface layer of main target made of metal Material etc.) efficiently remove.
According to the formational situation of the combination situation of the grafting material of the surface layer of target, especially metal layer, need to make The hydraulic pressure of water jet increases (for example, increasing to 90MPa or more), by the way that main target made of metal is made, even if to The water of high hydraulic pressure is collided, can also be removed grafting material in the case where not damaging target itself.
Hereinafter, enumerating the embodiment of the present invention, the present invention will be described in detail, but the present invention is not limited by embodiment below System.
Embodiment
Embodiment 1
(280 DEG C) are heated by the bonding layer to used sputtering target, to detach target from backer board.
It should be noted that for the sputtering target, in the state of before use, with the welding material (solder layer of In Thickness:350 μm) by the plate target (purity of aluminum:99.999%, Vickers hardness:15~17, size:2000mm× 200mm × 15mm) and anaerobic backer board (purity made of copper:99.99%, size:2300mm × 250mm × 15mm) engagement it is (right For the metallization of target, the welding material of Sn-Zn-In is used) and formed.
In turn, it wipes the welding material adhered on the joint surface of separated target off with the scraper of organosilicon, to the greatest extent may be used It can ground recycling welding material.After backer board separation, target is cut into 300mm × 200mm × 15mm or so.
The use of be equipped with nozzle diameter is 0.25mm (SUGINO MACHINE LIMITED systems, model:DN-0825), 0.30mm (SUGINO MACHINE LIMITED systems, model:DN-0830) each 3 of nozzle (totally 6, in the outside of nozzle head Configure 0.30mm nozzles at 3,0.25mm nozzles configured inside 3) circular nozzle head (SUGINO MACHINE LIMITED systems, model:MNH-2506CH), entire surface (hydraulic pressure is cleaned to the joint surface of target and sputter face injection water: 245MPa, water:11.6L/min, the distance between target and nozzle head:55mm, scanning:It 2 times, is overlapped (overlap):5mm, The rotary speed of nozzle head:1500min-1, the movement speed of nozzle head:3000mm/min).At this point, with the central shaft of nozzle head The mode vertical with the joint surface of used target configures nozzle head and used target, makes nozzle head along used target The long side direction of material scans (since the face of this side of the injection water of nozzle head is formed as downwardly projecting chevron structure, thus nozzle Towards relative to the inclined direction in joint surface, water collides joint surface from inclined direction).Engagement is removed from the target material surface after cleaning Material and metal layer become pear skin shape.Utilize UV, visible light near infrared spectrometer (Hitachi High- Technologies Corporation systems, U-4100 types) measure have become pear skin shape joint surface wavelength 300nm~ Normal reflection rate in 1500nm entire scopes.Using 5 ° of normal reflection auxiliary equipments, the incident light that incidence angle is 5 ° is irradiated to sample, Every the wavelength of the incident light of 100nm, the reflectivity relative to incident light with the reflected light of 5 ° of angle of reflection is found out.Entering When the wavelength for penetrating light is 1300nm, reflectivity is maximum, is 0.4%, and when the wavelength of incident light is 500nm, reflectivity is 0.3%, when the wavelength of incident light is 1000nm, reflectivity 0.2%.It should be noted that for being attached with before processing For the normal reflection rate in wavelength 300nm~1500nm entire scopes on the joint surface of grafting material, in the wavelength of incident light For 1300nm when, normal reflection rate is maximum, is 2~3% or so, when the wavelength of incident light is 500nm, normal reflection rate is 1~ 2%, when the wavelength of incident light is 1000nm, normal reflection rate is 1~2%.In addition, using contact surface roughness meter (Mitutoyo Corporation systems, SURFTEST SJ-301), utilizes method, needle specified in JIS B 0601 (2001) 3 points on the joint surface to having become pear skin shape measure arithmetic average roughness Ra, as a result, the average value of Ra is 19 μm.It needs Illustrate, 1.7 μm of the arithmetic average roughness Ra average out on the joint surface for being attached with grafting material before processing.
Use EDXRF analytical equipments (EDX-700L, detection limit of Shimadzu Seisakusho Ltd.:It is about 0.01 weight for In Measure %), the joint surface of the used target after cleaning is analyzed (semi-quantitative analysis) under the following conditions.As a result, In the joint surface of used target after cleaning, Sn, Zn, In from welding material and the Cu from backer board are complete Fail to detect.At this point, the element of the ingredient for grafting material, backer board, also to whether detecting that X-ray peak has carried out really Recognize.
It should be noted that according to mode similar to the above using EDXRF connecing to the used target before cleaning When conjunction face is analyzed, Sn, Zn, In from welding material are respectively with 10 weight % or less, 10 weight % or less, 1 weight % The amount of~70 weight % exists, and the Cu from backer board exists with the amount of 1 weight of weight %~50 %, it is known that utilizes the present invention's Cleaning method so that the used target after cleaning does not include substantially contained in the impurity from welding material and backer board Element.
< analysis conditions >
X-ray bombardment diameter:φ10mm
Excitation voltage:10kV (Na~Sc), 50kV (Ti~U)
Electric current:100μA
Minute:200 seconds (being measured 100 seconds under each excitation voltage)
Atmosphere:He
Pipe ball:Rh targets
Filter:Nothing
Assay method:Fundamental parameters method
Detector:Si (Li) semiconductor detector
Used target after cleaning is melted, is carried out in an atmosphere in 850 DEG C by (about 0.03Torr) under vacuum Stirring, except after removing dross, being cooled down in an atmosphere, manufacture as a result, recycles ingot casting.
For recycling the amount for the impurity for including in ingot casting, using GDMS (VG Elemental corporations, VG9000), the micro-analysis for Sn, Zn, In, Cu is carried out.By its result and using same method by used target The analysis result of ingot casting and not used target (before engagement) that (before cleaning) makes is shown in table 1 below together.
&#91;Table 1&#93;
Embodiment 2
(280 DEG C) are heated by the bonding layer to used sputtering target, to detach target from backer board.
It should be noted that for the sputtering target, in the state of before use, with the welding material (solder layer of In Thickness:350 μm) by anaerobic plate target (purity made of copper:99.99%, Vickers hardness:90, size:2000mm× 200mm × 15mm) and anaerobic backer board (purity made of copper:99.99%, size:2300mm × 250mm × 15mm) engagement it is (right For the metallization of target, the welding material of Sn-Zn-In is used) and formed.
In turn, it wipes the welding material adhered on the joint surface of separated target off with the scraper of organosilicon, to the greatest extent may be used It can ground recycling welding material.After backer board separation, target is cut into 300mm × 200mm × 15mm or so.
The use of be equipped with 6 nozzle diameters is 0.30mm (SUGINO MACHINE LIMITED systems, model:DN-0830) Nozzle circular nozzle head (SUGINO MACHINE LIMITED systems, model:MNH-2506CH), to the engagement of target Face injection water cleans entire surface (hydraulic pressure:245MPa, water:13.7L/min, the distance between target and nozzle head:25mm, Scanning:It 3 times, is overlapped (overlap):5mm, the rotary speed of nozzle head:1500cm-1, the movement speed of nozzle head:100mm/ min).At this point, configuring nozzle head and used target in such a way that the central shaft of nozzle head is vertical with joint surface, make nozzle head Long side direction along used target scans (since the face of this side of the injection water of nozzle head is formed as downwardly projecting chevron knot Structure, thus nozzle is towards relative to the inclined direction in joint surface, water collides joint surface from inclined direction).From the target after cleaning Surface removes grafting material and metal layer, becomes pear skin shape.It measures under the condition that is similarly to Example 1 and has become pear skin shape Joint surface the normal reflection rate in wavelength 300nm~1500nm entire scopes, as a result, incident light wavelength be 1300nm When, normal reflection rate is maximum, is 0.5%, and when the wavelength of incident light is 500nm, normal reflection rate is 0.1%, in the wave of incident light When a length of 1000nm, normal reflection rate is 0.3%.It should be noted that for the joint surface for being attached with grafting material before processing The normal reflection rate in wavelength 300nm~1500nm entire scopes for, incident light wavelength be 1300nm when, normal reflection Rate becomes maximum, is 2~3% or so, and when the wavelength of incident light is 500nm, normal reflection rate is 1~2%, in the wave of incident light When a length of 1000nm, normal reflection rate is 1~2%.In addition, measuring arithmetic average roughness in the way of similarly to Example 1 Ra, as a result, the average value of Ra is 17 μm.It should be noted that the arithmetic on the joint surface for being attached with grafting material before processing is flat Equal 2.1 μm of roughness Ra average out to.
It is under the condition that is similarly to Example 1, right using the EDXRF analytical equipments (EDX-700L) of Shimadzu Seisakusho Ltd. It is analyzed on the joint surface of used target after cleaning.As a result, on the joint surface of used target after cleaning, come It is not detected completely from Sn, Zn, In of welding material.
The joint surface of the used target before cleaning is analyzed using EDXRF according to mode similar to the above When, Sn, Zn, In from welding material respectively with 1 weight of weight %~20 %, 1 weight of weight %~20 %, 2 weight %~ The amount of 60 weight % exists.
(about 0.03Torr) under vacuum makes the used target after cleaning melt, carries out in an atmosphere in 1200 DEG C Stirring, except after removing dross, being cooled down in an atmosphere, manufacture as a result, recycles ingot casting.
For recycling the amount for the impurity for including in ingot casting, using GDMS (VG Elemental corporations, VG9000), the micro-analysis for Sn, Zn, In is carried out.Its result (is connect with using same method by not used target Before conjunction) analysis result of ingot casting that makes is shown in table 2 together.
&#91;Table 2&#93;
Although according to shown in table 2 as a result, confirm using cleaning after used target manufacture recycling ingot casting In include the amount of impurity (In, Sn, Zn from welding material) had increased slightly compared with not used target (before engagement), but The summation of its increments is the left and right 1.4ppm (on the basis of weight).
Embodiment 3
(280 DEG C) are heated by the bonding layer to used sputtering target, to detach target from backer board.
It should be noted that for the sputtering target, in the state of before use, with following welding material (solders The thickness of layer:350 μm) by the plate target (purity of aluminum:99.999%, Vickers hardness:15~17, size:2000mm× 200mm × 15mm) and anaerobic backer board (purity made of copper:99.99%, size:2300mm × 250mm × 15mm) it engages and shape At.
In turn, it wipes the welding material adhered on the joint surface of separated target off with the scraper of organosilicon, to the greatest extent may be used It can ground recycling welding material.After backer board separation, target is cut into 300mm × 200mm × 15mm or so.
The joint surface of target is cleaned under conditions of condition 1~10 below.In either case, from cleaning Target material surface afterwards eliminates grafting material and metal layer to become pear skin shape.For the target after cleaning, island is used Tianjin makes made EDXRF analytical equipments (EDX-700L, detection limit:For In be about 0.01 weight %), with implementation Under the conditions of example 1 is same, the joint surface of the used target after cleaning is analyzed.As a result, using after cleaning Target joint surface on, In, Sn, Zn from welding material and the Cu from backer board are not detected completely.Especially Ground, for the used target after the cleaning that is obtained under conditions of condition 1~8 below, under vacuum (for example, 0.03Torr), so that target is melted in 850 DEG C, be stirred in an atmosphere, after removing removing dross, cooled down in an atmosphere, by This, manufacture recycling ingot casting.
Using GDMS (VG Elemental corporations, VG9000), measure respectively not used target (before engagement), this again The amount for the impurity for including in cycle ingot casting and the ingot casting made by used target (before cleaning) using same method.It will knot Fruit is shown in table 3,4 below.
Condition 1
The welding material of engagement:In
The welding material of metallization:Sn-Zn-In
Hydraulic pressure:200MPa
Water:8.5L/min
Number of nozzle:6 (nozzle head uses the model MNH-2506CH of SUGINO MACHINE LIMITED)
Nozzle diameter:0.25mm (SUGINO MACHINE LIMITED systems, model:DN-0825)
Nozzle distance:25mm
Rotary speed:1500min-1
Movement speed:1000mm/min
Line (line) processing:1 time
It is overlapped (overlap):5mm
Cleaning treatment:Joint surface
Condition 2
The welding material of engagement:In
The welding material of metallization:Sn-Zn-In
Hydraulic pressure:200MPa
Water:8.5L/min
Number of nozzle:6 (nozzle head uses the model MNH-2506CH of SUGINO MACHINE LIMITED)
Nozzle diameter:0.25mm (SUGINO MACHINE LIMITED systems, model:DN-0825)
Nozzle distance:25mm
Rotary speed:1500min-1
Movement speed:1000mm/min
Line processing:1 time
It is overlapped (overlap):22mm
Cleaning treatment:Joint surface and sputter face
Condition 3
The welding material of engagement:In
The welding material of metallization:Sn-Zn-In
Hydraulic pressure:200MPa
Water:8.5L/min
Number of nozzle:6 (nozzle head uses the model MNH-2506CH of SUGINO MACHINE LIMITED)
Nozzle diameter:0.30mm (SUGINO MACHINE LIMITED systems, model:DN-0830)
Nozzle distance:25mm
Rotary speed:1500min-1
Movement speed:1000mm/min
Line processing:1 time
It is overlapped (overlap):22mm
Cleaning treatment:Joint surface and sputter face
Condition 4
The welding material of engagement:In
The welding material of metallization:Sn-Zn-In
Hydraulic pressure:200MPa
Water:8.5L/min
Number of nozzle:6 (nozzle head uses the model MNH-2506CH of SUGINO MACHINE LIMITED)
Nozzle diameter:0.25mm (SUGINO MACHINE LIMITED systems, model:DN-0825)
Nozzle distance:25mm
Rotary speed:1500min-1
Movement speed:2000mm/min
Line processing:2 times
It is overlapped (overlap):22mm
Cleaning treatment:Joint surface and sputter face
Condition 5
The welding material of engagement:In
The welding material of metallization:Sn-Zn-In
Hydraulic pressure:200MPa
Water:8.5L/min
Number of nozzle:6 (nozzle head uses the model MNH-2506CH of SUGINO MACHINE LIMITED)
Nozzle diameter:0.25mm (SUGINO MACHINE LIMITED systems, model:DN-0825)
Nozzle distance:25mm
Rotary speed:1500min-1
Movement speed:2000mm/min
Line processing:2 times
It is overlapped (overlap):5mm
Cleaning treatment:Joint surface and sputter face
Condition 6
The welding material of engagement:Sn-Zn
The welding material of metallization:Sn-Zn-In
Hydraulic pressure:200MPa
Water:8.5L/min
Number of nozzle:6 (nozzle head uses the model MNH-2506CH of SUGINO MACHINE LIMITED)
Nozzle diameter:0.25mm (SUGINO MACHINE LIMITED systems, model:DN-0825)
Nozzle distance:25mm
Rotary speed:1500min-1
Movement speed:1000mm/min
Line processing:2 times
It is overlapped (overlap):5mm
Cleaning treatment:Joint surface and sputter face
Condition 7
The welding material of engagement:In
The welding material of metallization:Sn-Zn-In
Hydraulic pressure:245MPa
Water:11.6L/min
Number of nozzle:6 (nozzle head uses the model MNH-2506CH of SUGINO MACHINE LIMITED)
Nozzle diameter:0.25mm, 0.30mm (each 3 of the nozzle of two kinds of diameters, SUGINO MACHINE LIMITED's Model DN-0825, DN-0830 configures 0.30mm nozzles at the outside of nozzle head 3, and 0.25mm nozzles are configured inside 3)
Nozzle distance:55mm
Rotary speed:1500min-1
Movement speed:4000mm/min
Line processing:2 times
It is overlapped (overlap):5mm
Cleaning treatment:Joint surface and sputter face
Condition 8
The welding material of engagement:Sn-Zn
The welding material of metallization:Sn-Zn-In
Hydraulic pressure:245MPa
Water:11.6L/min
Number of nozzle:6 (nozzle head uses the model MNH-2506CH of SUGINO MACHINE LIMITED)
Nozzle diameter:0.25mm, 0.30mm (each 3 of the nozzle of two kinds of diameters, SUGINO MACHINE LIMITED's Model DN-0825, DN-0830 configures 0.30mm nozzles at the outside of nozzle head 3, configures 0.25mm nozzles inside 3)
Nozzle distance:55mm
Rotary speed:1500min-1
Movement speed:3000mm/min
Line processing:2 times
It is overlapped (overlap):5mm
Cleaning treatment:Joint surface and sputter face
Condition 9
The welding material of engagement:In
The welding material of metallization:Sn-Zn-In
Hydraulic pressure:150MPa
Water:7.3L/min
Number of nozzle:3 (nozzle head is SUGINO MACHINE LIMITED systems, is configured in pitch circle (pitch Circle) diameter (P.C.D.) is the position of 20mm, along vertical direction injection water)
Nozzle diameter:0.35mm (SUGINO MACHINE LIMITED systems, model:DN-0835)
Nozzle distance:25mm
Rotary speed:1000min-1
Movement speed:1000mm/min
Line processing:1 time
It is overlapped (overlap):5mm
Cleaning treatment:Joint surface
Condition 10
The welding material of engagement:In
The welding material of metallization:Sn-Zn-In
Hydraulic pressure:245MPa
Water:3.4L/min
Number of nozzle:6 (nozzle head uses the model MNH-2506CH of SUGINO MACHINE LIMITED)
Nozzle diameter:0.15mm (SUGINO MACHINE LIMITED systems, model:DN-0815)
Nozzle distance:25mm
Rotary speed:1500min-1
Movement speed:1000mm/min
Line processing:1 time
It is overlapped (overlap):5mm cleaning treatments:Joint surface
&#91;Table 3&#93;
&#91;Table 4&#93;
Comparative example 1
Used plate target similarly to Example 1 is cut into 100mm × 200mm × 15mm or so, in room It is impregnated under temperature in the aqueous solution of nitric acid of 4.4wt% 20 hours, carries out the removal based on chemically treated welding material.Using with Embodiment 1 similarly handles and determines the normal reflection rate in wavelength 300nm~1500nm entire scopes on joint surface, knot Fruit, when the wavelength of incident light is 1300nm, normal reflection rate becomes maximum, is 13%, when the wavelength of incident light is 500nm, Normal reflection rate is 6.0%, and when the wavelength of incident light is 1000nm, normal reflection rate is 8.0%.In addition, according to same with embodiment 1 The mode of sample measures arithmetic average roughness Ra, as a result, the average value of Ra is 1.1 μm.It should be noted that before for processing It is attached with for the normal reflection rate in wavelength 300nm~1500nm entire scopes on the joint surface of grafting material, in incident light Wavelength when being 1300nm, normal reflection rate becomes maximum, is 2~3% or so, when the wavelength of incident light is 500nm, normal reflection Rate is 1~2%, and when the wavelength of incident light is 1000nm, normal reflection rate is 1~2%, the arithmetic average on the joint surface before processing 1.7 μm of roughness Ra average out to.Use EDXRF analytical equipments (EDX-700L, detection limit of Shimadzu Seisakusho Ltd.:For In Speech is about 0.01 weight %), under the condition that is similarly to Example 1, to the joint surface of the used target after chemical treatment It is analyzed.As a result, on the joint surface of used target after chemical processing, detect that 0.6wt%'s comes from backer board Cu, show to fail to remove impurity.
In addition, under vacuum (about 0.03Torr), in 850 DEG C, making the used target after chemical treatment melt, big It is stirred in gas, except after removing dross, being cooled down in an atmosphere, manufacture as a result, recycles ingot casting.
Using GDMS (VG Elemental corporations, VG9000), not used target (before engagement) is measured respectively, is compared The amount for the impurity for including in the recycling ingot casting of example 1, the ingot casting for making used target (before chemical treatment) melt and making.It will As a result it is shown in table 5 below.
&#91;Table 5&#93;
For only having carried out the comparative example 1 of the processing based on acid, although handle within 20 hours, recycling casting The total amount for the impurity (that is, In, Sn, Zn, Cu) from grafting material and backer board for including in ingot is about with weight basis 19ppm fails to obtain the recycling ingot casting with the composition substantially identical with original target.
Embodiment 4
(280 DEG C) are heated by the bonding layer to used sputtering target, to detach target from backer board.
It should be noted that for the sputtering target, with following welding material (thickness of solder layer:350 μm) it will Plate target (the purity of aluminum:99.999%, Vickers hardness:14~17, size:2000mm × 200mm × 15mm) and nothing Oxygen backer board (purity made of copper:99.99%, size:2300mm × 250mm × 15mm) it engages and is formed.
In turn, it wipes the welding material adhered on the joint surface of separated target off with the scraper of organosilicon, to the greatest extent may be used It can ground recycling welding material.By target after backer board separation, target is cut into 300mm × 200mm × 15mm or so.
Joint surface, sputter face and the side of pair 55 targets are cleaned under conditions of condition 11 below.For appointing For one target, grafting material and metal layer are eliminated to become pear skin shape from the target material surface after cleaning.From clear In 55 after washing randomly choose 10, under the condition that is similarly to Example 1, measure have become pear skin shape joint surface Normal reflection rate in wavelength 300nm~1500nm entire scopes.For any target, maximum normal reflection rate is 0.4% Left and right, when wavelength is 500nm, normal reflection rate average out to 0.2% or so, when wavelength is 1000nm, normal reflection rate average out to 0.2% or so.The arithmetic average roughness Ra for 10 targets selected at random, knot are measured using method similarly to Example 1 The average value of fruit, Ra is 20 μm.It should be noted that for the joint surface for being attached with grafting material before processing in wavelength For normal reflection rate in 300nm~1500nm entire scopes, when the wavelength of incident light is 1300nm, normal reflection rate becomes most Greatly, it is 2~3% or so, when the wavelength of incident light is 500nm, normal reflection rate is 1~2%, is in the wavelength of incident light When 1000nm, normal reflection rate is 1~2%, 1.8 μm of the arithmetic average roughness Ra average out on the joint surface before processing.For clear Target after washing uses EDXRF analytical equipments (EDX-700L, detection limit of Shimadzu Seisakusho Ltd.:It is about 0.01 for In Weight %), under the condition that is similarly to Example 1, the joint surface of the used target after 55 cleanings is analyzed.Knot Fruit, on the joint surface of used target after cleaning, In, Sn, Zn from welding material and the Cu from backer board are equal It is not detected completely.In addition, finding out yield rate by the weight difference before and after the cleaning of 55 targets, as a result, average out to 98%.
Next, in a vacuum, in 800 DEG C, 25 (about 50kg) in the target cleaned for making to be handled are molten Change, after removing removing dross, molten metal is injected into the mold of carbon in an atmosphere, in an atmosphere cools down molten metal, by This, manufacture recycling ingot casting.Using GDMS (VG Elemental corporations, VG9000 (model)), measure in recycling ingot casting Including impurity amount.Show the result in table 4.
Condition 11
The welding material of engagement:In
The welding material of metallization:Sn-Zn-In
Hydraulic pressure:245MPa
Water:18.6L/min
Number of nozzle:6 (nozzle head (is sprayed using the model MNH-2506-15C of SUGINO MACHINE LIMITED Mouth is configured at the position of P.C.D.36mm))
Nozzle diameter:0.35mm (SUGINO MACHINE LIMITED systems, model:DN-0835)
Nozzle distance:60mm
Rotary speed:2000min-1
Movement speed:4000mm/min
Line processing:2 times
It is overlapped (overlap):5mm
Cleaning treatment:Joint surface, sputter face and side
Industrial availability
Through the invention, such as by using above-mentioned device, in the manner described above to used target it cleans, The used target for not including the element from grafting material and supporting member substantially can be obtained.In addition, by in this way Used target manufacture ingot casting for raw material, the recycling with the composition substantially identical with original target can be obtained and cast Ingot.Through the invention, the target with the composition substantially identical with original target can be regenerated using such recycling ingot casting Therefore material is useful for the recycling of target.

Claims (13)

1. the cleaning method of target, the cleaning method includes following processes:
From with grafting material by main target made of metal and supporting member in conjunction with and described in being detached in the sputtering target of formation The process of target;And
By the face injection water for being attached with the grafting material to the target, to by the grafting material from the target The process of removing.
2. the cleaning method of target as described in claim 1, wherein the pressure of the water is 90MPa or more.
3. the cleaning method of target as claimed in claim 1 or 2, wherein the metal is aluminium or copper.
4. the manufacturing method of target, the manufacturing method includes following processes:Implement described in any one of claims 1 to 33 Cleaning method.
5. target, which is characterized in that its be from grafting material will main target made of metal and supporting member in conjunction with and The target detached in the sputtering target of formation, also,
It can't detect the element from grafting material and supporting member by energy dispersion type x-ray fluorescence analysis.
6. recycling the manufacturing method of ingot casting, the manufacturing method includes following processes:By to implementing claims 1 to 3 The target of the cleaning method is cast, to obtain including the recycling ingot casting of the metal.
7. recycle ingot casting, come use by oneself grafting material by main target made of metal and supporting member in conjunction with and formation The target of sputtering target, in the recycling ingot casting,
The total amount of element from the grafting material and supporting member is less than 10ppm with weight basis.
8. as claimed in claim 7 recycling ingot casting, wherein as it is described recycling ingot casting principal component metal be aluminium or Copper.
9. recycling ingot casting as claimed in claim 7, which is characterized in that the metal of the principal component as the recycling ingot casting Total amount for aluminium, the impurity is less than 5ppm with weight basis.
10. device, described device is used for:To from grafting material will main target made of metal and supporting member in conjunction with and The face injection water for being attached with the grafting material of the target detached in the sputtering target of formation, thus by the grafting material It is removed from the target,
Described device includes:
It is used at least one nozzle head to the jet port of the target injection water at least one;
Actuator for operating the nozzle head;And
Process chamber for configuring the actuator, storage the target and handled.
11. device as claimed in claim 10, described device further include:For the target to be fixed in the process chamber Fixture.
12. the device as described in claim 10 or 11, described device further include:Tipper for making the target overturning Structure.
13. the device as described in any one of claim 10~12, described device includes drainage mechanism, and the drainage mechanism is used In the water sprayed from the jet port is recycled and is drained, the processed material of the grafting material removed from the target will be included Separation.
CN201810267287.2A 2017-03-30 2018-03-28 Target cleaning method, the device for it, target manufacturing method and target and recycling ingot casting manufacturing method and recycling ingot casting Pending CN108690958A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113275545A (en) * 2021-05-26 2021-08-20 江阴恩特莱特镀膜科技有限公司 Cooler for casting target material and cooling method

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113245249A (en) * 2021-05-08 2021-08-13 宁国九鼎橡塑制品有限公司 Air conditioner clutch driving-disc brushing device

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002053953A (en) * 2000-08-04 2002-02-19 Tosoh Corp Method for manufacturing sputtering target
JP2008149297A (en) * 2006-12-20 2008-07-03 Kn Lab Analysis:Kk Exfoliating/cleaning apparatus
CN101509127A (en) * 2008-02-15 2009-08-19 爱发科材料股份有限公司 Method for manufacturing sputtering target, method for cleaning sputtering target, sputtering target and sputtering device
US20170009336A1 (en) * 2014-03-31 2017-01-12 Kabushiki Kaisha Toshiba Method of manufacturing sputtering target and sputtering target
CN106334686A (en) * 2015-07-07 2017-01-18 宁波江丰电子材料股份有限公司 Cleaning method of target material composite

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4286076B2 (en) * 2003-06-30 2009-06-24 三井金属鉱業株式会社 Recycled target material and target material recycling method
JP4270971B2 (en) * 2003-07-24 2009-06-03 三井金属鉱業株式会社 Manufacturing method of sputtering target
CN106282938B (en) * 2015-05-13 2018-11-27 宁波创润新材料有限公司 The method for recycling target

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002053953A (en) * 2000-08-04 2002-02-19 Tosoh Corp Method for manufacturing sputtering target
JP2008149297A (en) * 2006-12-20 2008-07-03 Kn Lab Analysis:Kk Exfoliating/cleaning apparatus
CN101509127A (en) * 2008-02-15 2009-08-19 爱发科材料股份有限公司 Method for manufacturing sputtering target, method for cleaning sputtering target, sputtering target and sputtering device
US20170009336A1 (en) * 2014-03-31 2017-01-12 Kabushiki Kaisha Toshiba Method of manufacturing sputtering target and sputtering target
CN106334686A (en) * 2015-07-07 2017-01-18 宁波江丰电子材料股份有限公司 Cleaning method of target material composite

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
罗立强等: "《X射线荧光光谱仪》", 31 January 2008, 化学工业出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113275545A (en) * 2021-05-26 2021-08-20 江阴恩特莱特镀膜科技有限公司 Cooler for casting target material and cooling method

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