CN104066700A - Ceramic cylindrical sputtering target and method for producing same - Google Patents

Ceramic cylindrical sputtering target and method for producing same Download PDF

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Publication number
CN104066700A
CN104066700A CN201380006061.2A CN201380006061A CN104066700A CN 104066700 A CN104066700 A CN 104066700A CN 201380006061 A CN201380006061 A CN 201380006061A CN 104066700 A CN104066700 A CN 104066700A
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China
Prior art keywords
sputtering target
target material
cylindrical sputtering
ceramic cylindrical
target
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Granted
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CN201380006061.2A
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Chinese (zh)
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CN104066700B (en
Inventor
真崎贵则
石田新太郎
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Mitsui Mining and Smelting Co Ltd
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Mitsui Mining and Smelting Co Ltd
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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    • 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
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    • C23C14/34—Sputtering
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    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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    • B28—WORKING CEMENT, CLAY, OR STONE
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    • B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
    • B28B11/24—Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
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Abstract

The present invention provides a ceramic cylindrical sputtering target characterized in being a single article having a length of 500 mm or longer and a relative density of 95% or greater. The ceramic cylindrical sputtering target is a single article having a high density and length of 500 mm or longer and therefore eliminates the need to use a stack of multiple sputtering targets in order to obtain a long target. Consequently, when the ceramic cylindrical sputtering target of the present invention is used in a magnetron rotary cathode sputtering target, and the like, there are no or few partitions in the target as a whole and therefore there is little arcing and particle generation during sputtering.

Description

Ceramic cylindrical sputtering target material and manufacture method thereof
Technical field
The present invention relates to a kind of ceramic cylindrical sputtering target material and manufacture method thereof, more specifically, relate to ceramic cylindrical sputtering target material and the manufacture method thereof of a kind of high-density and long size.
Background technology
Magnetron-type rotating cathode sputter equipment is, inner side at cylindrical target has magnetic field generation device, carry out from the inner side of target the device that cooling one side rotates target and carries out sputter on one side, and make the whole surface of target even thereby quilt is cut by acid etching (erosion).Therefore, be 20～30% with respect to the service efficiency of plate-type magnetron sputter equipment, magnetron rotating cathode sputter equipment can obtain more than 60% very high service efficiency.And due to compared with existing plate-type magnetron sputter equipment, by making target rotation, thereby per unit area can be inputted larger power, therefore can obtain higher film forming speed.
In recent years, for the glass substrate that makes to use in flat-panel monitor or solar cell maximizes, and form film on this substrate having maximized, and need length to exceed the cylindrical target of the long size of 3m.
Such rotating cathode sputter mode be easy to be processed in the metallic target that drum and physical strength are stronger extensively universal.But, because the intensity of ceramic target is lower and more crisp, therefore in manufacturing processed, easily crack, distortion etc.Therefore,, although can produce the round shape target of short size in ceramic target, cannot produce the round shape target of the long size of better performances.
At patent documentation 1, a kind of following technology is disclosed,, in the cylindrical target that the round shape target of short size is carried out to stacking and long size that produce, each target is engaged as benchmark by the outer surface taking cylindrical target, and the difference of height of the cutting part place generation of target is made as below 0.5mm, thereby suppress the electric arc or the particulate that produce because of difference of height.But, due in this technology, in the situation that round shape target is shorter, if multiple targets are not carried out stackingly, cannot obtain the cylindrical target of long size, therefore the quantity that makes the cutting part producing between target and target is increased.As long as there is cutting part, even if there is not difference of height, also cannot avoid causing because of cutting part the generation of electric arc.Therefore, in a large amount of described technology that produce of quantity of cutting part, the generation increased frequency of electric arc.In addition, owing to will concentrate in cutting part place electric discharge in sputter, therefore, in a fairly large number of situation of cutting part, in sputter, easily produce the crackle taking cutting part as starting point.In the time that multiple targets are engaged, expend time in, and it is also poor to manufacture upper efficiency.
A kind of following technology is disclosed in patent documentation 2,, in the sintering of the ceramic sintered bodies of hollow cylinder shape, by described ceramic molding being placed on the tabular ceramic molding with the sintering shrinkage identical with the sintering shrinkage of ceramic molding and carrying out sintering, thereby the crackle while preventing sintering, obtains more than 95% sintered compact of relative density.But, even also can there are the following problems in this technology,,, in the case of ceramic powder being carried out to moulding, degreasing and sintering and producing the cylinder ceramic sintered bodies that length is long size more than 500mm, in any one operation in moulding, degreasing or sintering, all can crack.
Patent documentation 3 discloses and has a kind ofly utilized sputtering process and produce the technology of length for ITO round shape target more than 500mm.But, utilize sputtering process and the round shape target that obtains cannot be established highlyer by relative density, and relative density mostly is 70～80% most.In the time implementing sputter with the lower target of relative density, the number of times that electric arc produces will increase.Therefore,, in the time using the long size round shape target being obtained by sputtering process to implement sputter, the number of times that electric arc produces will increase.
Formerly technical literature
Patent documentation
Patent documentation 1: TOHKEMY 2010-100930 communique
Patent documentation 2: TOHKEMY 2005-281862 communique
Patent documentation 3: Japanese kokai publication hei 10-68072 communique
Summary of the invention
Invent problem to be solved
The object of the invention is to, the ceramic cylindrical sputtering target material of a kind of high-density and long size is provided.
Solve the method for problem
Even if the inventor finds that formed body is for long size, also can not crack in the mill, the manufacture method of the ceramic cylindrical sputtering target material of distortion etc., and successfully produce the ceramic cylindrical sputtering target material of high-density and long size.
That is, the present invention is a kind of ceramic cylindrical sputtering target material, it is characterized in that, described ceramic cylindrical sputtering target material is that length is more than 500mm and relative density is more than 95% body component.
More than the length of described ceramic cylindrical sputtering target material is preferably 750mm, more preferably more than 1000mm, more preferably more than 1500mm.
Described ceramic cylindrical sputtering target material for example can adopt, and the content of Sn is with SnO 2amount is scaled the tin indium oxide system of mass percent 1～10%, and the content of Al is with Al 2o 3amount is scaled the zinc oxide system of the aluminium doping of mass percent 0.1～5%, or the content of In is with In 2o 3the content that amount is scaled mass percent 40～60%, Ga is with Ga 2o 3amount is scaled the content of mass percent 20～40%, Zn and measures the indium gallium zinc oxide system that is scaled mass percent 10～30% with ZnO.
In addition, the present invention is a kind of ceramic cylindrical sputtering target, it is characterized in that, by grafting material, described ceramic cylindrical sputtering target material is engaged with backing pipe.
In addition, the present invention is a kind of manufacture method of ceramic cylindrical sputtering target material, comprising: operation 1, prepare particle by the slurries that contain ceramic material powder and organic additive; Operation 2, thus it carries out CIP moulding to described particle and produces columnar formed body; Operation 3, it carries out degreasing to described formed body; And operation 4, the formed body of described degreasing is carried out to sintering, the manufacture method of described ceramic cylindrical sputtering target material is characterised in that, in described operation 1, the amount of described organic additive is mass percent 0.1～1.2% with respect to the amount of described ceramic material powder.
In the manufacture method of described ceramic cylindrical sputtering target material, be preferably, described organic additive contains tackiness agent, and this tackiness agent is, and the polymerization degree is 200～400 and the basicity molar percentage polyvinyl alcohol that is 60～80%.
Invention effect
Because ceramic cylindrical sputtering target material of the present invention is a body component with length more than 500mm, thereby therefore adopt long size to use without stacking multiple sputtering target materials.Therefore, owing to use ceramic cylindrical sputtering target material of the present invention in magnetron rotating cathode sputter equipment etc. in the situation that, do not have cutting part or its comparatively small amt in overall target, therefore in sputter, the generation of electric arc or particulate is less.In addition, because ceramic cylindrical sputtering target material density of the present invention is high, therefore in sputter, the generation of electric arc is less.
The manufacture method of ceramic cylindrical sputtering target material of the present invention can effectively be manufactured the described ceramic cylindrical sputtering target material of sening as an envoy to and not crack, is out of shape.
The mode carrying out an invention
< ceramic cylindrical sputtering target material >
Ceramic cylindrical sputtering target material of the present invention is integrated parts, and the length of described ceramic cylindrical sputtering target material is more than 500mm and relative density is more than 95%.One body component not refers to by multiple component and forms, but the parts that overall target is not cut apart as object.By stacking multiple target parts or engage and form target be not a body component.Therefore, ceramic cylindrical sputtering target material of the present invention be different from by stacking multiple round shape targets or engage and form length be round shape target more than 500mm.
Ceramic cylindrical sputtering target material of the present invention for example, can be manufactured by the manufacture method of narrating hereinafter.
As mentioned above, because the intensity of ceramic target is lower and more crisp, therefore in existing sintering process, in manufacturing processed, can crack, distortion etc., thereby cannot produce the ceramic cylindrical sputtering target material that length is a body component more than 500mm.Therefore, in the prior art, the tubular sputtering target material that multiple length must be less than to the short size of 500mm connects, thereby forms the tubular sputtering target material of long size.Due in the time adopting such structure, the quantity that produces cutting part between target and target increases, therefore in the time implementing sputter with the target with this structure, by the increased frequency that causes that because of this cutting part electric arc produces.
Due to ceramic cylindrical sputtering target material of the present invention long body that be integrated and that there is length more than 500mm, therefore without multiple targets are connected to form long body.Ceramic cylindrical sputtering target material of the present invention, according to needed length, can only be implemented sputter with one, also many connections can be carried out to sputter in addition.Due in the situation that only implementing sputter with one, there is not cutting part, therefore can not produce the electric arc causing because of cutting part.Due in the situation that many connections are implemented to sputter, the tubular sputtering target material that forms it also has length more than 500mm, therefore can become the length of utilizing less just to achieve the goal.Therefore,, owing to comparing the comparatively small amt of cutting part with the situation that the target of many short sizes is connected to the tubular sputtering target material that forms long size, the generation number of times of the electric arc therefore causing because of cutting part is less.
Although can produce the ceramic cylindrical sputtering target material of long size one and that there is length more than 500mm in existing spraying method, utilize spraying method and the relative density of the round shape target that obtains is higher, be 70～80%.Therefore, in the time using the round shape target being obtained by spraying method to implement sputter, the generation increased frequency of electric arc.Because the relative density of ceramic cylindrical sputtering target material of the present invention is more than 95%, compared with the round shape target therefore obtaining with utilizing spraying method, the number of times that produces electric arc when sputter is less.
The length of ceramic cylindrical sputtering target material of the present invention is more than 500mm, more than being preferably 750mm, more preferably more than 1000mm, more preferably more than 1500mm.Implement in the situation of sputter with a target of the present invention, target is more long more can large-area film forming, can not produce the electric arc causing because of cutting part.Due in the situation that many targets of the present invention are connected to implement sputter, adopt the more long length that more can just achieve the goal with less radical of target, and can reduce the quantity of cutting part, therefore can reduce the generation number of times of the electric arc causing because of cutting part.
Although the upper limit of the length to ceramic cylindrical sputtering target material of the present invention is restriction especially not, due to the restriction of magnetron rotating cathode sputter equipment etc., and make length on be limited to about 3400mm.
More than the internal diameter of ceramic cylindrical sputtering target material of the present invention is preferably 100mm.In the time being internal diameter as above, by rotating cathode sputter mode film forming effectively.
Out of roundness, cylindricity and the vibration tolerance of ceramic cylindrical sputtering target material of the present invention are preferably in 1mm, more preferably in 0.5mm, more preferably in 0.1mm.Due to out of roundness, cylindricity and the more difficult generation of the less electric arc of vibration tolerance, therefore preferred.
The relative density of ceramic cylindrical sputtering target material of the present invention is more than 95%, is preferably more than 99%, more preferably more than 99.5%.The relative density of target is higher, the crackle of the target that thermal shocking, the temperature head etc. more can prevent because of sputter time causes, thus can not waste and effectively utilize target thickness.In addition, can reduce the generation of particulate and electric arc, thereby obtain good membranous.Although to the not restriction especially of the upper limit of described relative density, be generally 100%.
Material, ceramic kind to ceramic cylindrical sputtering target material of the present invention are not particularly limited, can list, for example, Indium sesquioxide tin protoxide class material (ITO), aluminum oxide one added zinc oxide based material (AZO) and Indium sesquioxide gallium monoxide one added zinc oxide based material (IGZO) etc.
In the situation that pottery is ITO, the content of the Sn in this target is with SnO 2amount converts and is preferably mass percent 1～10%, more preferably mass percent 2～10%, more preferably mass percent 3～10%.In the time that the content of Sn is in described scope, target has low-resistance advantage.
In the situation that pottery is AZO, the content of the Al in this target is with Al 2o 3amount converts and is preferably mass percent 0.1～5%, more preferably mass percent 1～5%, more preferably mass percent 2～5%.In the time that the content of Al is in described scope, target has low-resistance advantage.
In the situation that pottery is IGZO, be preferably, the content of the In in this target is with In 2o 3amount is scaled mass percent 40～60%, and the content of Ga is with Ga 2o 3amount is scaled mass percent 20～50%, and the content of Zn is scaled mass percent 5～30% with ZnO amount, and more preferably, the content of In is with In 2o 3amount is scaled mass percent 40～55%, and the content of Ga is with Ga 2o 3amount is scaled mass percent 25～35%, and the content of Zn is scaled mass percent 15～30% with ZnO amount, and more preferably, the content of In is with In 2o 3amount is scaled mass percent 40～50%, and the content of Ga is with Ga 20 3amount is scaled mass percent 25～35%, and the content of Zn is scaled mass percent 20～30% with ZnO amount.In the time that the content of In, Ga and Zn is in described scope, has advantages of by sputter and obtain good TFT (thin film transistor: ThinFilm Transistor) characteristic.
< ceramic cylindrical sputtering target >
Ceramic cylindrical sputtering target of the present invention is by grafting material, described ceramic cylindrical sputtering target material to be engaged and formed with backing pipe.
Described backing pipe has the drum that ceramic cylindrical sputtering target material can be engaged conventionally.To the not restriction especially of the kind of backing pipe, can from existing used backing pipe, suitably select to use according to target.For example, as the material of backing pipe, can exemplify out stainless steel, titanium etc.
Kind to described grafting material is also not particularly limited, and can from existing used jointing material, suitably select to use according to target.For example, as jointing material, can exemplify out the scolder of indium system etc.
One of ceramic cylindrical sputtering target material can be engaged in the outside of a backing pipe, also two can be bonded on same axis above abreast.By in two above situations about engaging abreast, gap between each ceramic cylindrical target, the length of cutting part is generally 0.05～0.5mm, is preferably 0.05～0.3mm, more preferably 0.05mm.Although when the shorter sputter of length of cutting part, electric arc is more not easy to produce, and in the time being less than 0.05mm, likely because of the thermal expansion in engaging process, in sputter procedure, and makes target collide each other, break.
Method of joining is not particularly limited, can adopts the method identical with existing ceramic cylindrical sputtering target material.
The manufacture method > of < ceramic cylindrical target
The manufacture method of ceramic cylindrical sputtering target material of the present invention, comprising: operation 1, prepare particle by the slurries that contain ceramic material powder and organic additive; Operation 2, produces columnar formed body thereby described particle is carried out to CIP moulding; Operation 3, carries out degreasing to described formed body; And operation 4, the formed body of described degreasing is carried out to sintering, the manufacture method of described ceramic cylindrical sputtering target material is characterised in that, in described operation 1, the amount of described organic additive is mass percent 0.1～1% with respect to the amount of described ceramic material powder.
By this manufacture method, can effectively manufacture the described ceramic cylindrical sputtering target material of the present invention of sening as an envoy to and not crack, be out of shape.
In this manufacture method, be preferably, described organic additive contains tackiness agent, this tackiness agent is polyvinyl alcohol, the polymerization degree of described polyvinyl alcohol be 200～400 and basicity molar percentage be 60～80%.
(operation 1)
In operation 1, prepare particle by the slurries that contain ceramic material powder and organic additive.
By preparing particle by ceramic material powder and organic additive, and this particle is offered to the CIP moulding of operation 2, thereby can obtain making the fillibility of raw material to improve and highdensity formed body.In addition, fill uneven difficult generation and can fill uniformly.Punching press inequality is also not easy to occur.
Ceramic material powder is to produce the ceramic powder as the structured material of target by this manufacture method.
For example, in the situation that pottery is ITO, as ceramic material powder, can use In 2o 3powder and SnO 2the mixed powder of powder, can use separately ito powder, or and In 2o 3powder and SnO 2powder mixes use.Utilize BET (Brunauer-Emmett-Teller) method to measure In 2o 3powder, SnO 2the specific surface area of powder and ito powder is respectively 1～40m conventionally 2/ g.In 2o 3powder, SnO 2the mixture ratio of powder and ito powder is the mode in described scope and being appropriately determin with the content of the Constitution Elements in this target.In this manufacture method, by In 2o 3powder and SnO 2in the situation that the mixed powder of powder uses as ceramic material powder, confirm the SnO in ceramic material powder 2the content (mass percent %) of powder can be regarded as, with the SnO in the final target being obtained 2the content (mass percent %) of the Sn that amount converts.
In the situation that pottery is AZO, as ceramic material powder, can use Al 2o 3the mixed powder of powder and ZnO powder, can use separately AZO powder, or and Al 2o 3powder and ZnO powder mix use.Utilize BET method to measure Al 2o 3the specific surface area of powder, ZnO powder and AZO powder is respectively 1～40m conventionally 2/ g.Al 2o 3the mixture ratio of powder, ZnO powder and AZO powder is the mode in described scope and suitably being determined with the content of structural element in this target.In this manufacture method, by Al 2o 3in the situation that the mixed powder of powder and ZnO powder uses as ceramic material powder, confirm the Al in ceramic material powder 2o 3the content (mass percent %) of powder is regarded as, with in the final target being obtained with Al 2o 3the content (mass percent %) of the Al that amount converts.
In the situation that pottery is IGZO, as ceramic material powder, can use In 2o 3powder, Ga 2o 3the mixed powder of powder and ZnO powder, can use separately IGZO powder, or and In 2o 3powder, Ga 2o 3powder and ZnO powder mix use.Utilize BET method to measure In 2o 3powder, Ga 2o 3the specific surface area of powder, ZnO powder and IGZO powder is respectively 1～40m conventionally 2/ g.In 2o 3powder, Ga 2o 3the mixture ratio of powder, ZnO powder and IGZO powder is the mode in described scope and suitably being determined with the content of structural element in this target.In this manufacture method, by In 2o 3powder, Ga 2o 3in the situation that the mixed powder of powder and ZnO powder uses as ceramic material powder, confirm the In in ceramic material powder 2o 3powder, Ga 2o 3the content (mass percent %) of powder and ZnO powder is regarded as respectively, with in the final target being obtained with In 2o 3amount convert In content (mass percent %), with Ga 2o 3the content (mass percent %) of the Zn that measures the content (%) of the Ga converting and convert with ZnO amount.
In the time using the ceramic material powder that mixes the different two or more powder of particle diameter and obtain, due to the particle doped with the less powder of particle diameter between the particle of the larger powder of particle diameter, the density therefore with molding uprises, the strengthened advantage of sintered compact.
Blending means to powder is not particularly limited, and for example, each powder and zirconium white spheroid can be inserted in cylindrical shell, carries out ball mill mixing.
Described organic additive is, for the suitable material that regulates the proterties of slurries, molding and add.As organic additive, can exemplify out tackiness agent, dispersion agent and softening agent etc.
In operation 1, the amount of organic additive is mass percent 0.1～1.2% with respect to the amount of ceramic material powder, is preferably mass percent 0.2～1.0%, more preferably mass percent 0.4～0.8%.When the described combined amount of organic additive is during more than mass percent 1.2%, the strength decreased degree that appears at sometimes the formed body in skimming processes becomes the situation that produces greatly and easily degreasing cracking, thereby the emptying aperture appearing at sometimes in degreasing aftershaping body increases the situation that is difficult to densification.In the time that the described combined amount of organic additive is less than mass percent 0.1%, there is sometimes the sufficient effect that cannot obtain each composition.In the time that the combined amount of organic additive is set in above-mentioned scope, it is more than 500mm can producing length and relative density is the ceramic cylindrical sputtering target material of more than 95% conduct one body component.
Tackiness agent is bonding for the ceramic material powder of formed body is carried out, thereby the intensity of raising formed body is added.As tackiness agent, can use obtain formed body in known powder sintering time and common used tackiness agent.
Wherein, be preferably polyvinyl alcohol (PVA), and be preferably, the polymerization degree be 200～400 and basicity be the polyvinyl alcohol of molar percentage 60～80%.In the time using such tackiness agent, even if the addition of tackiness agent is a small amount of, also can in the time of CIP moulding, prepare and hold yielding particle, be filled with densely the formed body that is not easy cracking of ceramic material powder by CIP moulding, its result is can produce and can not make crackle, the high-density of distortion generation and the ceramic cylindrical target of long size.For example, when the combined amount of organic additive is set in above-mentioned scope, and while using described tackiness agent, can stably produce length is that 750mm is above, relative density is the ceramic cylindrical target of more than 95% body component.
Generally, when by the operation of moulding, degreasing and sintering, when ceramic powder is made into the ceramic cylindrical target of longer size, crackle can produce in any operation of moulding, degreasing and sintering.Therefore,, in existing manufacture method, cannot produce length is that 500mm is above, relative density is the ceramic cylindrical target of more than 95% body component.When at CIP formed body, crackle when moulding becomes long size, when large-scale, and the crackle can think moulding time causes greatly because screen resilience becomes.The in the situation that of cast molding body, can think because of moisture inequality, particulate segregation be that starting point ftractures.Although can eliminate the situation of moulding crackle as long as increase amount of binder, in the time of increase amount of binder, cylinder formed body embrittlement in degreasing or sintering process and breaking.In addition, because the too much tackiness agent of interpolation can become tackiness agent segregation and the starting point of degreasing cracking, so not preferred.
In manufacture method of the present invention, by using described tackiness agent, even if grow the formed body of size, also can obtain being not easy by adding a small amount of tackiness agent the formed body of cracking, therefore in degreasing and sintering process, cylinder formed body is difficult for breaking.That is, when using when described tackiness agent, moulding, degreasing and burn till in any operation in be all not easy to crack, can stably obtain the ceramic cylindrical target of long size.
Can think by using described tackiness agent, can obtain such effect is based on following reason.
For example, in the case of the slurries that contain raw material powder, tackiness agent and water are dried to prepare by spraying particle, slurries are sprayed and made the outer side shifting of water to drop by dry in the drop that forms, meanwhile make raw material powder and tackiness agent also to the outer side shifting of drop.Water volatilizees outward at drop, and its result is that raw material powder and tackiness agent be aggegation densely on drip gauge face, and forms the particle with hard tunicle.Because raw material powder, tackiness agent and water move and make this particle become hollow at peripheral part, therefore this hollow bulb is negative pressure.Make particle depression in order to eliminate this pressure difference.Because the particle of such depression is harder, therefore not yielding in the time of moulding.Therefore, not densification of formed body can be produced, and the large defect of the starting point of cracking can be become.Can think, such situation is the major cause that produces the situation of cracking in the time making the formed body of long size.
In the time of the lower tackiness agent of to use the polymerization degree be 200～400 the polymerization degree, can obtain as the high molecular complexing of the composition of tackiness agent less, and lower slurries of viscosity.When using, tackiness agent is fixed and when the lower tackiness agent of the polymerization degree, can be produced the slurries that raw material powder concentration is high with low viscosity than being made as.Therefore, because the movement of the water in drop in the time that slurries are sprayed is less, therefore granule interior is difficult to form hollow, and is difficult to depression.Because the complexing of tackiness agent in particle is less, therefore the bonding force of tackiness agent a little less than, thereby particle is easily out of shape.In addition,, in the time that the slurries of high density are sprayed, because raw material powder and tackiness agent can not aggegations at the surface element of drop, therefore surface element is difficult to become fine and close, thereby makes the intensity step-down of particle.According to such reason, can think and can obtain by CIP moulding the formed body that is not easy to break that is filled with densely ceramic material powder.
In addition,, in the time of the lower tackiness agent of to use basicity be molar percentage 60～80% basicity, in the slurries that formed by raw material powder, tackiness agent and water, the hydrophobic grouping of tackiness agent is adsorbed on powder, thereby can obtain dispersed higher slurries.Due in the time that the temperature with more than cloud point is sprayed slurries, tackiness agent is separated out at short notice, and not to the outer side shifting of drop, therefore on whole particle, under the dispersed state that has tackiness agent, be dried, thereby can obtain the particle that surface element intensity is lower.According to such reason, can think and can obtain by CIP moulding the formed body that is filled with densely ceramic material powder.
As mentioned above, although be a less side as the polymerization degree and the basicity of the polyvinyl alcohol of tackiness agent, can obtain yielding particle.Therefore, be preferably, as the polymerization degree of the polyvinyl alcohol of tackiness agent, below 400, basicity is that molar percentage is below 80%.On the other hand, when the polymerization degree and basicity are when too small, the formed body obtaining will become too softness and operability will decline.Therefore, be preferably, as the polymerization degree of the polyvinyl alcohol of tackiness agent, more than 200, basicity is that molar percentage is more than 60%.More preferably, be molar percentage 250～350% as the polymerization degree of the polyvinyl alcohol of tackiness agent, basicity is molar percentage 65～75%, and more preferably, the polymerization degree is molar percentage 280～320, and basicity is molar percentage 68～72%.
Addition as the polyvinyl alcohol of tackiness agent is preferably mass percent 0.1～1.0%, more preferably mass percent 0.1～0.65%, more preferably mass percent 0.1～0.3% with respect to ceramic material powder.The addition of polyvinyl alcohol is more, the higher moulding of plasticity-more becomes and is not easy cracking, and the strength decreased degree that occurs sometimes the formed body in skimming processes becomes the situation that produces greatly and easily degreasing cracking, thereby occur that sometimes degreasing aftershaping body hollow hole increases the situation that is not easy to densification that becomes.Therefore, described scope is preferred.
Dispersion agent is, for improving the raw material powder of slurries and the dispersiveness of tackiness agent is added.As dispersion agent, can list, such as poly carboxylic acid ammonium, ammonium polyacrylate etc.
Softening agent is to add for the plasticity-that improves formed body.As softening agent, can list for example polyoxyethylene glycol (PRG), ethylene glycol (EG) etc.
Contain ceramic material powder and organic additive in preparation slurries time the dispersion medium that uses be not particularly limited, can be from water according to object, in alcohol etc., suitably select to use.
In the method for the slurries that contain ceramic material powder and organic additive in preparation, be not particularly limited, for example, can use ceramic material powder, organic additive and dispersion medium are put into tank, carry out the method for ball mill mixing.
In the method for being prepared particle by slurries, be not particularly limited, for example, can use spray-drying process, rotate comminution granulation, extruder grain method etc.Wherein, higher in the mobility of particle, when moulding, easily produce the aspect of easily deformable particle, be preferably spray-drying process.Condition for spray-drying process is not particularly limited, and can suitably select common used condition in the granulation of ceramic material powder to implement.
(operation 2)
In operation 2, the particle of being prepared by operation 1 is carried out to CIP moulding (Cold IsostaticPressing (cold isostatic compaction)) and produces columnar formed body.In the time producing formed body by CIP moulding, can obtain density homogeneous and directivity less, even if implement degreasing and burn till also the columnar formed body of long size not easy to crack.
As the model using in CIP moulding, can produce the model of the columnar formed body of normally used in CIP moulding, long size, for example, can use urethanes of having upper and lower sealable lid and columned core (axle) etc.
Pressure when CIP moulding is generally 800kgf/cm 2above, be preferably 1000kgf/cm 2above, 3000kgf/cm more preferably 2above.Pressure is larger, filler particles more densely, thus can make formed body densification and high strength.Upper limit of pressure value during for CIP moulding is not particularly limited, and is generally 5000kgf/cm 2.
While decompression after pressurizeing in CIP moulding process, pressure is at 200kgf/cm 2in following scope, preferably decompression rate is made as to 200kgf/cm 2below h, more preferably decompression rate is made as to 100kgf/cm 2below h, further preferably decompression rate is made as to 50kgf/cm 2below h.Due at 200kgf/cm 2in decompression in following scope, the screen resilience producing on formed body is stronger, and therefore formed body easily breaks.When decompression rate is made as to 200kgf/cm 2when h is following, screen resilience dies down, and formed body is difficult for breaking.In the time that the decompression rate with such is implemented decompression, can stably produce the ceramic cylindrical target of high-density and long size.For example, when using described tackiness agent, the combined amount of organic additive is located in described scope, and while adopting described decompression rate, can stably produce length and be the above and relative density of 1000mm is the ceramic cylindrical target of more than 95% body component.Lower value to decompression rate is not particularly limited, and is generally 30kgf/cm 2.
To pressure higher than 200kgf/cm 2scope in decompression rate be not particularly limited, be generally 200～1000kgf/cm 2h.
(operation 3)
In operation 3, the formed body being produced by operation 2 is carried out to degreasing.Degreasing is by heating and implement formed body.
Skimming temp is generally 600～800 DEG C, is preferably 700～800 DEG C, more preferably 750～800 DEG C.Although the intensity of the higher formed body of skimming temp is higher, due in the time exceeding 800 DEG C, can cause the contraction of formed body, be therefore preferably at 800 DEG C and carry out below degreasing.
Degreasing time is generally 3～10 hours, is preferably 5～10 hours, more preferably 10 hours.Although the intensity of the longer formed body of degreasing time is higher, because the heating by 10 hours roughly completes degreasing, also can not improve even if therefore degreasing time is made as to the intensity that exceedes 10 hours formed bodys.
Heat-up rate in the temperature range that reaches 400 DEG C, be preferably 50 DEG C/below h, more preferably 30 DEG C/below h, more preferably 20 DEG C/below h.Due to when carry out degreasing till reaching 400 DEG C, and skimming processes high speed while heating up, formed body becomes and is easy to break, and is therefore preferably, and reaches till 400 DEG C with 50 DEG C/low speed below h and heats up.In the time heat-up rate being located in described scope, can be stably to produce the ceramic cylindrical target of high-density and long size.For example, when using described tackiness agent, the combined amount of organic additive is located in described scope, and the decompression rate during by CIP moulding is located in described scope, and heat-up rate during by degreasing is while being located at described scope, can stably produce length and be the ceramic cylindrical target of above and more than 95% body component of relative density of 1500mm.Because degreasing in the temperature higher than more than 400 DEG C completes, therefore in order to shorten process period, can be at faster speed, for example heat up in 50 DEG C/h left and right.
(operation 4)
In operation 4, in operation 3 and carried out sintering by the formed body of degreasing.
Calcining furnace is not particularly limited, can uses existing used calcining furnace in the manufacture of ceramic target.
In the situation that pottery is ITO, sintering temperature is generally 1450～1700 DEG C, is preferably 1500～1650 DEG C, more preferably 1550～1600 DEG C.In the situation that pottery is AZO or IGZO, be generally 1250～1500 DEG C, be preferably 1300～1450 DEG C, more preferably 1350～1400 DEG C.More can obtain highdensity target although sintering temperature is more high, when too high, break making the sintering structure hypertrophyization of target and becoming easily.
Sintering time is generally 3～30 hours, is preferably 5～10 hours, more preferably 5～8 hours.Although the easier densification of the longer target of sintering time, when long, breaks making the sintering structure hypertrophyization of target and becoming easily.
Heat-up rate is generally 100～500 DEG C/h.Cooling rate is generally 10～100 DEG C/h, is preferably 10～50 DEG C/h, more preferably 10～30 DEG C/h.More be not easy to produce because of the poor caused crackle of thermal stresses although cooling rate is more little, be less than that 10 DEG C/h thermal stresses is poor also can not be changed conventionally even if be made as.
Calcining atmosphere is not particularly limited, is generally atmospheric atmosphere or oxygen atmosphere.
The sintered compact obtaining is used as sputtering target material by the processing of the necessity such as enforcement machining and uses.
Embodiment
The evaluation method of the sputtering target material obtaining in embodiment and comparative example is as described below.
1. relative density
The relative density of sputtering target material is measured based on Archimedes's method.Particularly, the aerial weight of sputtering target material, divided by volume (the water proportion in the water of=sputtering target sintered compact in weight/measurement temperature), and is made as to relative density with respect to the percentile value of the theoretical density ρ (g/cm3) based on following mathematical expression (X).(unit: %).
[mathematical expression 1]
&rho; &equiv; [ C 1 / 100 &rho; 1 + C 2 / 100 &rho; 2 + . . . + C i / 100 &rho; i ] - 1 . . . ( X )
(in mathematical expression (X), C 1～C irepresent respectively the content (weight percent %) of the structural material of target, ρ 1～ρ irepresent and C 1～C idensity (the g/cm of each corresponding structural material 3)).
2. the evaluation of the cracking of sputtering target material or formed body
By visual observation sputtering target material and formed body, unconfirmed to occurring being evaluated as " A " in the situation of crackle on sputtering target material or formed body, in situation about confirming, be evaluated as " B ".
< ITO target >
[embodiment 1]
Be 10m by the specific surface area of measuring by BET method 2the SnO of/g 2powder and the specific surface area of measuring by BET method are 10m 2the In of/g 2o 3powder is so that SnO 2the amount mode that becomes mass percent 1% mix, and carry out ball mill mixing by zirconia ball in tank, thereby prepare ceramic material powder.
In this tank, as tackiness agent, add the polyvinyl alcohol (polymerization degree: 280 of mass percent 0.1% for ceramic material powder, basicity is molar percentage 68%), as dispersion agent, add the poly carboxylic acid ammonium of mass percent 0.3% for ceramic material powder, and as dispersion medium, add the water of mass percent 15% for ceramic material powder, carry out ball mill mixing and prepare slurries.Ratio with respect to the amount of the ceramic material powder of the total amount (total amount of polyvinyl alcohol amount and poly carboxylic acid ammonium amount) of organic additive is mass percent 0.4%.
These slurries are supplied in spray drying unit, are 10000rpm at atomization rotating speed, and temperature in is under the condition of 250 DEG C, to implement spraying to be dried to prepare particle.
The internal diameter that described particle is rapped while be filled in the columned core (axle) that has upper and lower sealable lid and have external diameter 165mm is in the urethanes model of 210mm (wall thickness is 10mm), the length drum that is 1219mm, and after rubber cast is airtight, with 800kgf/cm 2pressure carry out CIP moulding, thereby produce columnar formed body.Decompression rate after CIP moulding is higher than 200kgf/cm 2pressure range in be made as 300kgf/cm 2h, lower than 200kgf/cm 2scope in be made as 200kgf/cm 2h.The length of the formed body obtaining is 1212mm.
This formed body is heated to degreasing.Skimming temp is 700 DEG C, and degreasing time is 10 hours, and heat-up rate is made as 20 DEG C/h in the scope that reaches 400 DEG C, is made as 50 DEG C/h in the scope higher than 400 DEG C.
The formed body of degreasing is carried out to sintering, thereby produce sintered compact.Be sintered to, in atmospheric atmosphere, sintering temperature is made as 1600 DEG C, and sintering time is made as 10 hours, and heat-up rate is made as 300 DEG C/h, and cooling rate is made as 50 DEG C/h.
Obtained sintered compact is carried out to machining, is 155mm thereby produce external diameter, and internal diameter is 135mm, the ITO tubular sputtering target material that length is 1000mm.
Be 133mm by In solder bonds at external diameter by three described targets, internal diameter is 123mm, on the SUS304 backing pipe processed that length is 3200mm, thereby produces ITO target.Interval (length of cutting part) between each target is made as 0.2mm.
Table 1 is for representing the relative density of target, and the evaluation of the crackle of target and formed body.
[embodiment 2～20, comparative example 1～9]
Implement embodiment 2～20 and comparative example 1～9 according to following condition.
By the SnO in ceramic material powder 2the addition of the content of powder, the polymerization degree of polyvinyl alcohol and basicity and polyvinyl alcohol, the addition of poly carboxylic acid ammonium are made as the condition shown in table 1, in addition implement in mode similarly to Example 1, thereby prepare particle.
This particle is carried out to CIP moulding, thereby produce the columnar formed body with the length shown in table 1.In CIP moulding, embodiment 2,3,9～18, comparative example 6 use the urethanes model identical with embodiment 1, and relate to other embodiment and comparative example, use has core and the internal diameter identical with the urethanes model using in embodiment 1, and has the urethanes type of the length of the formed body that can obtain length as shown in table 1.By after CIP moulding, 200kgf/cm 2decompression rate in following pressure range is made as the condition shown in table 1.CIP condition of molding is in addition identical with embodiment 1.In comparative example 5, in molding procedure, on formed body, produce crackle.
The formed body not cracking in molding procedure is heated to degreasing.The heat-up rate reaching in the temperature range of 400 DEG C is made as to the condition shown in table 1, and degreasing condition is in addition identical with embodiment 1.In comparative example 1～4 and 8～9, in degreasing process, on formed body, produce crackle.
With the condition identical with embodiment 1 in degreasing process, do not crack carried out sintering by the formed body of degreasing, thereby produce sintered compact.Obtained sintered compact is carried out to machining, thereby produce the ITO tubular sputtering target material with the external diameter shown in table 1, internal diameter and length.
In order to obtain the quantity of the cutting part shown in table 1, be 133mm and the described target of many (more than the radicals of one of the quantity of cutting part) is bonded on to external diameter by In scolder, internal diameter is 123mm, on the SUS304 backing pipe processed that length is 3200mm, thereby produces ITO target.Interval (length of cutting part) between each target is made as 0.2mm.
Table 1 is for representing the relative density of each target that obtains and the evaluation of the crackle of target and formed body.
< AZO target >
[embodiment 21]
Be 5m by the specific surface area of measuring by BET method 2the Al of/g 2o 3powder and the specific surface area of measuring by BET method are 10m 2the ZnO powder of/g is so that Al 2o 3the content mode that becomes mass percent 0.5% mix, and carry out ball mill mixing by zirconia ball in tank, thereby prepare ceramic material powder.
Except using this ceramic material powder, implement in mode similarly to Example 1, prepare particle.
Under the condition identical with embodiment 1, the internal diameter that use has upper and lower sealable lid and has a columned core (axle) that external diameter is 167mm is the urethanes model of 213mm (wall thickness 10mm), the length drum that is 1233mm, this particle is carried out to CIP moulding, thereby produce the columnar formed body with the length shown in table 2.
Under the condition identical with embodiment 1, this formed body is carried out to degreasing.
Under the condition identical with embodiment 1 to being carried out sintering by the formed body of degreasing, thereby produce sintered compact.To obtained sintered compact machining, thereby produce the AZO tubular sputtering target material with the external diameter shown in table 2, internal diameter and length.
Be 133mm by In solder bonds at external diameter by three described targets, internal diameter is 123mm, on the SUS304 backing pipe processed that length is 3200mm, thereby produces AZO target.Interval (length of cutting part) between each target is made as 0.2mm.
Table 2 is for representing the evaluation of the relative density of target and the crackle of target and formed body.
[embodiment 22～33, comparative example 10～18]
Implement embodiment 22～33 and comparative example 10～18 according to following condition.
By the Al in ceramic material powder 2o 3the content of powder, the polymerization degree of polyvinyl alcohol and basicity, and the addition of the addition of polyvinyl alcohol and poly carboxylic acid ammonium is made as the condition that table 2 represents, implements in addition, thereby prepare particle in mode similarly to Example 21.
This particle is carried out to CIP moulding, thereby produce the round shape formed body with length shown in table 2.In CIP moulding, in embodiment 22,28～30,33, comparative example 14 processes, use the urethanes identical with embodiment 21, relate to other embodiment and comparative example, use has core and the internal diameter identical with the urethanes using in embodiment 21, and has the urethanes of the length of the formed body that can obtain length as shown in table 2.By after CIP moulding, 200kgf/cm 2decompression rate in following pressure range is made as the condition shown in table 2.The condition of CIP moulding is in addition made as identical with embodiment 21.In comparative example 13, in molding procedure, on formed body, produce crackle.
The formed body not cracking in molding procedure is heated to de-ester.The heat-up rate reaching in the temperature range of 400 DEG C is made as to condition shown in table 2, and degreasing condition is in addition made as identical with embodiment 21.In comparative example 10～12 and 16～18, in degreasing process, on formed body, produce crackle.
To be carried out sintering to what do not produce slight crack in degreasing process by the formed body of degreasing under the condition identical with embodiment 21, thereby produce sintered compact.Obtained sintered compact is carried out to machining, thereby produce the AZO tubular sputtering target material with the external diameter shown in table 2, internal diameter and length.
In order to obtain the quantity of cutting part shown in table 2, be 133mm and many (more than the radical of one of the quantity of cutting part) described targets are bonded on to external diameter by In scolder, internal diameter is 123mm, on the SUS304 backing pipe processed that length is 3200mm, thereby produces AZO target.Interval (length of cutting part) between each target is made as 0.2mm.
Table 2 is for representing the relative density of each target obtaining, and the evaluation of the crackle of target and formed body.
< IGZO target >
[embodiment 34]
Be 10m by the specific surface area of measuring by BET method 2the In of/g 2o 3powder and the specific surface area of measuring by BET method are 10m 2the Ga of/g 2o 3powder and the specific surface area of measuring by BET method are 10m 2the ZnO powder of/g is so that In 2o 3the content of powder becomes mass percent 44.2%, Ga 2o 3the content of powder is mass percent 29.9%, and the content of ZnO powder is that the mode of mass percent 25.9% is mixed, and carries out ball mill mixing by zirconia ball in tank, thereby prepares ceramic material powder.
Except using this ceramic material powder, and the replacement polyvinyl alcohol (polymerization degree: 280, basicity side's molar percentage 68%) and use the polyvinyl alcohol (polymerization degree: 500, basicity is molar percentage 90%) in addition, implement according to the mode identical with embodiment 1, thereby prepare particle.
The internal diameter that use has upper and lower sealable lid and has a columned core (axle) that external diameter is 171mm is the urethanes of 218mm (heavy wall), the length drum that is 653mm, except by after CIP moulding, 200kgf/cm 2decompression rate in following pressure range is made as 300kgf/cm 2beyond h, under the condition identical with embodiment 1, this particle is carried out to CIP moulding, thereby produce the columnar formed body with length shown in table 3.
Under the condition identical with embodiment 1, this formed body is carried out to degreasing.
Under the condition identical with embodiment 1 to being carried out sintering by the formed body of degreasing, thereby produce sintered compact.Obtained sintered compact is carried out to machining, thereby produce the IGZO tubular sputtering target material with the external diameter shown in table 3, internal diameter and length.
By In scolder, target described in the six roots of sensation being bonded on to external diameter is 133mm, and internal diameter is 123mm, on the SUS304 backing pipe processed that length is 3200mm, thereby produces IGZO target.Interval (length of cutting part) between each target is made as 0.2mm.
Table 3 is for representing the relative density of target, and the evaluation of the crackle of target and formed body.
[embodiment 35～44, comparative example 19～25]
Embodiment 35～44 and comparative example 19～25 are carried out according to following condition.
By the In in ceramic material powder 2o 3the content of powder, Ga 2o 3the polymerization degree and the basicity of the content of powder and the content of ZnO powder, polyvinyl alcohol, and the addition of the addition of polyvinyl alcohol and poly carboxylic acid ammonium is made as the condition shown in table 3, the mode same with embodiment 34 implemented in addition, thereby prepares particle.
This particle is carried out to CIP moulding, thereby produce the round shape formed body with length shown in table 3.In CIP moulding, in embodiment 35～36, comparative example 19～20,22～25 processes, use the urethanes identical with embodiment 34, and relate to other embodiment and comparative example, use has core and the internal diameter identical with the urethanes using in embodiment 34, and has the urethanes of the length of the formed body that can obtain length as shown in table 2.By after CIP moulding, 200kgf/cm 2decompression rate in following pressure range is made as condition shown in table 3.The condition of CIP moulding is in addition made as identical with embodiment 34.In comparative example 20, in molding procedure, on formed body, produce crackle.
The formed body that does not produce slight crack in molding procedure is heated to degreasing.The heat-up rate reaching in the temperature range of 400 DEG C is made as to the condition shown in table 3, and degreasing condition is in addition made as identical with embodiment 34.In comparative example 19 and 23～25, in degreasing process, on formed body, produce crackle.
What under the condition identical with embodiment 34, do not produce slight crack in to degreasing process is carried out sintering by the formed body of degreasing, thereby produces sintered compact.Obtained sintered compact is carried out to machining, thereby produce the IGZO tubular sputtering target material with the external diameter shown in table 3, internal diameter and length.
In order to obtain the quantity of cutting part shown in table 3, by In scolder, many (more than the radical of of the quantity of cutting part) described targets being bonded on to external diameter is 133mm, internal diameter is 123mm, on the SUS304 backing pipe processed that length is 3000mm, thereby produces IGZO target.Interval (length of cutting part) between each target is made as 0.2mm.
Table 3 is for representing the relative density of each target obtaining, and the evaluation of the crackle of target and formed body.
[table 1]
[table 2]
[table 3]
As shown in table 1～3, in the embodiment 1～44 that has implemented manufacture method of the present invention, can obtain a kind of following target,, in the making processes of target, do not produce the crackle of target and formed body, there is length more than 500mm and there is ITO tubular sputtering target material, AZO tubular sputtering target material or the IGZO tubular sputtering target material of more than 95% relative density and the target being formed by these.
Not in the comparative example of manufacture method of the present invention implementing, in the situation of the amount of organic additive with respect to the amount of ceramic material powder and more than mass percent 1.2%, in degreasing process, on formed body, crack, or the relative density of target, lower than in 95% situation, cracks in molding procedure on formed body.In comparative example, cannot produce the ceramic cylindrical sputtering target material that there is length more than 500mm and there is more than 95% relative density.

Claims (10)

1. a ceramic cylindrical sputtering target material, is characterized in that,
Described ceramic cylindrical sputtering target material is that length is more than 500mm and relative density is more than 95% body component.
2. ceramic cylindrical sputtering target material as claimed in claim 1, is characterized in that,
The length of described ceramic cylindrical sputtering target material is more than 750mm.
3. ceramic cylindrical sputtering target material as claimed in claim 1, is characterized in that,
The length of described ceramic cylindrical sputtering target material is more than 1000mm.
4. ceramic cylindrical sputtering target material as claimed in claim 1, is characterized in that,
The length of described ceramic cylindrical sputtering target material is more than 1500mm.
5. the ceramic cylindrical sputtering target material as described in any one in claim 1 to 4, is characterized in that,
The content that described ceramic cylindrical sputtering target material is Sn is with SnO 2amount is scaled the tin indium oxide system of mass percent 1～10%.
6. the ceramic cylindrical sputtering target material as described in any one in claim 1 to 4, is characterized in that,
The content that described ceramic cylindrical sputtering target material is Al is with Al 2o 3amount is scaled the zinc oxide system of the aluminium doping of mass percent 0.1～5%.
7. the ceramic cylindrical sputtering target material as described in any one in claim 1 to 4, is characterized in that,
The content that described ceramic cylindrical sputtering target material is In is with In 2o 3amount is scaled mass percent 40～60%, and the content of Ga is with Ga 2o 3amount is scaled mass percent 20～40%, and the content of Zn is scaled the indium gallium zinc oxide system of mass percent 10～30% with ZnO amount.
8. a ceramic cylindrical sputtering target material, is characterized in that,
By grafting material, the tubular sputtering target material described in any one in claim 1～7 is engaged on backing pipe and is formed.
9. a manufacture method for ceramic cylindrical sputtering target material, comprising:
Operation 1, prepares particle by the slurries that contain ceramic material powder and organic additive;
Operation 2, produces columnar formed body thereby described particle is carried out to CIP moulding;
Operation 3, carries out degreasing to described formed body; And
Operation 4, carries out sintering to the formed body of described degreasing,
The manufacture method of described ceramic cylindrical sputtering target material is characterised in that,
In described operation 1, the amount of described organic additive is mass percent 0.1～1.2% with respect to the amount of described ceramic material powder.
10. the manufacture method of ceramic cylindrical sputtering target material as claimed in claim 9, is characterized in that,
Described organic additive contains tackiness agent, and this tackiness agent is, the polymerization degree be 200～400 and basicity be the polyvinyl alcohol of molar percentage 60～80%.
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