CN104066700B - Ceramic cylindrical sputtering target material and its manufacture method - Google Patents

Ceramic cylindrical sputtering target material and its manufacture method Download PDF

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Publication number
CN104066700B
CN104066700B CN201380006061.2A CN201380006061A CN104066700B CN 104066700 B CN104066700 B CN 104066700B CN 201380006061 A CN201380006061 A CN 201380006061A CN 104066700 B CN104066700 B CN 104066700B
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sputtering target
target material
cylindrical sputtering
ceramic cylindrical
ceramic
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CN104066700A (en
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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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    • C04B35/453—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
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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Abstract

The present invention is a kind of ceramic cylindrical sputtering target material, it is characterised in that the ceramic cylindrical sputtering target material is, length be more than 500mm and relative density be more than 95% integrated component.As the ceramic cylindrical sputtering target material of the present invention is with high density and the integrated component of the length of more than 500mm, therefore multiple sputtering target materials stacking need not be used so as to be set to long size.Therefore, because used in magnetron rotating cathode sputter equipment etc. in the case of the ceramic cylindrical sputtering target material of the present invention, integrally there are no cutting part or its negligible amounts in target, therefore the generation of electric arc or microgranule is less in sputtering.

Description

Ceramic cylindrical sputtering target material and its manufacture method
Technical field
The present invention relates to a kind of ceramic cylindrical sputtering target material and its manufacture method, more specifically, are related to a kind of highly dense The ceramic cylindrical sputtering target material and its manufacture method of degree and long size.
Background technology
Magnetron-type rotating cathode sputter equipment is have magnetic field generation device in the inner side of cylindrical target, from target Inner side carry out cooling while the device for rotating target and being sputtered, and make the whole surface of target by acid etching (erosion) It is uniform so as to be cut.It is 20～30% accordingly, with respect to the service efficiency of plate-type magnetron sputter equipment, magnetron rotation is cloudy Pole sputter equipment can obtain more than 60% very high service efficiency.It is additionally, since and splashes with existing plate-type magnetron Injection device is compared, and is rotated by making target, so as to per unit area can be input into larger power, therefore, it is possible to obtain higher film forming Speed.
In recent years, it is in order that flat faced display or the glass substrate used in solaode maximize and big at this Thin film is formed on the substrate of type, and need cylindrical target of the length more than the long size of 3m.
It is wide in the stronger metallic target of drum and mechanical strength is easily processed into that such rotating cathode sputters mode General popularization.But, as the intensity of ceramic target is relatively low and more crisp, therefore easily cracks in the fabrication process, deform. Therefore, although the cylindrical shape target of short size can be produced in ceramic target, but the long chi of better performances cannot be produced Very little cylindrical shape target.
Patent document 1 discloses that a kind of following technology, i.e. stacked in the cylindrical shape target by short size and made In the cylindrical target of the long size made, by each target being engaged on the basis of the outer surface of cylindrical target, and by target Cutting part at the difference of height that produces be set to below 0.5mm, so as to the electric arc that suppresses to produce because of difference of height or microgranule.However, Due in the art, in the case where cylindrical shape target is shorter, being grown if not stacking to multiple targets The cylindrical target of size, therefore by the increasing number of the cutting part for making to produce between target and target.Simply by the presence of cutting part, then Even if there is no difference of height, cannot also avoid causing the generation of electric arc because of cutting part.Therefore, in the big volume production of quantity of cutting part In the raw technology, the generation increased frequency of electric arc.Further, since electric discharge will be concentrated in sputtering at cutting part, therefore Cutting part it is a fairly large number of in the case of, the crackle with cutting part as starting point is easily produced in sputtering.When entering to multiple targets The time is then expended during row engagement, and it is also poor to manufacture upper efficiency.
Patent Document 2 discloses a kind of following technology, i.e. in the sintering of the ceramic sintered bodies of hollow cylinder shape In, by the ceramic mouldings are placed in the tabular with the sintering shrinkage identical sintering shrinkage of ceramic mouldings On ceramic mouldings and it is sintered, so as to prevent crackle when sintering, obtains the sintered body of relative density more than 95%.So And, even if in the art also can there are the following problems, i.e. make ceramic powders are carried out with molding, defat and sintering It is in the case of going out the cylindrical ceramic sintered body of the long size that length is more than 500mm, any one in molding, defat or sintering Can crack in individual operation.
Patent document 3 discloses that a kind of utilization metallikon and produce the ITO cylindrical shape targets that length is more than 500mm Technology.But, relative density cannot be set higher by the cylindrical shape target obtained using metallikon, and relative density is up to 70～80%.When implementing sputtering when using the relatively low target of relative density, the number of times that electric arc is produced will increase.Therefore, when making When implementing sputtering with the long size cylindrical shape target by obtained from metallikon, the number of times that electric arc is produced will increase.
Citation
Patent documentation
Patent documentation 1：Japanese Unexamined Patent Publication 2010-100930 publications
Patent documentation 2：Japanese Unexamined Patent Publication 2005-281862 publications
Patent documentation 3：Japanese Unexamined Patent Publication 10-68072 publication
The content of the invention
Invent problem to be solved
It is an object of the present invention to provide the ceramic cylindrical sputtering target material of a kind of high density and long size.
The method for solving problem
The inventors discovered that even if molded body is long size, the ceramics that also will not be cracked in the mill, deform etc. are justified The manufacture method of tubular sputtering target material, and it is successfully fabricated out 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 characterised in that the ceramic cylindrical sputtering target material Be more than 500mm for, length and relative density be more than 95% integrated component.
The length of the ceramic cylindrical sputtering target material is preferably more than 750mm, more preferably more than 1000mm, further Preferably more than 1500mm.
The ceramic cylindrical sputtering target material can for example be adopted, and the content of Sn is with SnO2Amount is scaled mass percent 1 ～10% tin indium oxide system, the content of Al is with Al2O3Amount is scaled the Zinc Oxide of the aluminum doping of mass percent 0.1～5% System, or the content of In is with In2O3Amount is scaled the content of mass percent 40～60%, Ga with Ga2O3Amount is scaled quality hundred Divide the content than 20～40%, Zn that the indium gallium zinc oxide system of mass percent 10～30% is scaled with ZnO amounts.
Additionally, the present invention is a kind of ceramic cylindrical sputtering target, it is characterised in that will be the ceramics round by grafting material Tubular sputtering target material and backing pipe joint.
Additionally, the present invention is a kind of manufacture method of ceramic cylindrical sputtering target material, including：Operation 1, by former containing ceramics The serosity of feed powder end and organic additive is preparing granule；Operation 2, which carries out CIP molding so as to produce to the granule Columnar molded body；Operation 3, which carries out defat to the molded body；And operation 4, the molded body of the defat is carried out Sintering, the manufacture method of the ceramic cylindrical sputtering target material is characterised by, in the operation 1, the organic additive Amount relative to the ceramic material powder amount be mass percent 0.1～1.2%.
In the manufacture method of the ceramic cylindrical sputtering target material, preferably, the organic additive contains binding agent, The binding agent is, the degree of polymerization be 200～400 and basicity molar percentage be 60～80% polyvinyl alcohol.
Invention effect
Due to the integrated component that the ceramic cylindrical sputtering target material of the present invention is the length with more than 500mm, therefore nothing Multiple sputtering target materials need to be stacked so as to using long size to use.Therefore, because in magnetron rotating cathode sputter equipment etc. In the case of ceramic cylindrical sputtering target material using the present invention, there are no cutting part or its negligible amounts in target on the whole, Therefore in sputtering, the generation of electric arc or microgranule is less.Further, since the ceramic cylindrical sputtering target material density of the present invention is high, because This generation of electric arc in sputtering is less.
The manufacture method of the ceramic cylindrical sputtering target material of the present invention can effectively manufacture described ceramic cylinder of sening as an envoy to Shape sputtering target material is not cracked, is deformed.
The mode for carrying out an invention
<Ceramic cylindrical sputtering target material>
The ceramic cylindrical sputtering target material of the present invention is integrated part, and the length of the ceramic cylindrical sputtering target material is More than 500mm and relative density are more than 95%.Integrated component does not mean that and is made up of multiple parts, but target is integrally made For the part that object is not split.The target for stacking or engage and formed multiple target parts is not one portion Part.Therefore, ceramic cylindrical sputtering target material of the invention to be different from and stack multiple cylindrical shape targets or engage and formed Cylindrical shape target of the length for more than 500mm.
The ceramic cylindrical sputtering target material of the present invention for example, can pass through the manufacture method system for hereinafter being described Make.
As noted previously, as the intensity of ceramic target is relatively low and more crisp, therefore in existing sintering process, in manufacture process In can crack, deform, so as to the ceramic cylindrical sputtering target of the integrated component that length is more than 500mm cannot be produced Material.Therefore, in the prior art, it is necessary to by multiple length less than 500mm short size tubular sputtering target material connection, so as to Form the tubular sputtering target material of long size.Due to, when using such structure, cutting part being produced between target and target Increasing number, thus when using with the structure target come implement sputtering when, will cause because of the cutting part electric arc produce Increased frequency.
Due to the present invention ceramic cylindrical sputtering target material be integrated, and the length with more than 500mm long size Body, therefore multiple targets need not be connected to form long body.The ceramic cylindrical sputtering target material of the present invention is according to required Length, only can implement sputtering using one, in addition also can be by many connections being sputtered.Due to only being come using one In the case of implementing sputtering, there is no cutting part, therefore the electric arc caused because of cutting part will not be produced.Due to by many companies In the case of fetching enforcement sputtering, its tubular sputtering target material also length with more than 500mm is constituted, therefore, it is possible to become Using the less length for just achieving the goal.Therefore, because the circle of long size is formed with the target of many short sizes is connected The situation of tubular sputtering target material compares the negligible amounts of cutting part, thus the generation number of times of the electric arc caused because of cutting part compared with It is few.
Although one and the long size of the length with more than 500mm pottery can be produced in existing spraying process Porcelain tubular sputtering target material, but obtained from spraying process, the relative density of cylindrical shape target is higher, is 70～80%.Cause This, when implementing sputtering when using the cylindrical shape target by obtained from spraying process, the generation increased frequency of electric arc.Due to the present invention Ceramic cylindrical sputtering target material relative density be more than 95%, therefore with the cylindrical shape target phase obtained from spraying process Than the number of times that electric arc is produced during sputtering is less.
The present invention ceramic cylindrical sputtering target material length be more than 500mm, preferably more than 750mm, more preferably More than 1000mm, more preferably more than 1500mm.In the case of implementing to sputter using the target of a basic invention, target It is more long can large-area film forming, the electric arc caused because of cutting part will not be produced.Due at the targets that will be invented more at all Connection come in the case of implementing sputtering, the length that adopt target more long more just can be achieved the goal with less radical, and can subtracting The quantity of few cutting part, therefore, it is possible to reduce the generation number of times of the electric arc caused because of cutting part.
Although especially not limiting to the upper limit of the length of the ceramic cylindrical sputtering target material of the present invention, due to Restriction of magnetron rotating cathode sputter equipment etc., and make the upper limit of length be 3400mm or so.
The internal diameter of the ceramic cylindrical sputtering target material of the present invention is preferably more than 100mm.When for internal diameter as above when, Being capable of effectively film forming by way of rotating cathode sputtering.
Within the out of roundness of ceramic cylindrical sputtering target material of the present invention, cylindricity and vibration tolerance are preferably 1mm, more Within preferably 0.5mm, within more preferably 0.1mm.Due to out of roundness, cylindricity and the less electric arc of vibration tolerance more not It is also easy to produce, therefore preferably.
The relative density of the ceramic cylindrical sputtering target material of the present invention is more than 95%, preferably more than 99%, more preferably For more than 99.5%.The relative density of target is higher, the target for being more prevented from thermal shock when sputtering, temperature difference etc. and causing The crackle of material such that it is able to do not waste and effectively utilize its thickness.Furthermore it is possible to the generation of microgranule and electric arc is reduced, So as to obtain good film quality.Although especially not limiting to the upper limit of the relative density, usually 100%.
Material to the ceramic cylindrical sputtering target material of the present invention, i.e. ceramic species are not particularly limited, and can include, For example, Indium sesquioxide. tin monoxide class material (ITO), one added zinc oxide based material of aluminium oxide (AZO) and Indium sesquioxide. gallium monoxide one Added zinc oxide based material (IGZO) etc..
In the case where ceramics are for ITO, the content of the Sn in the target is with SnO2Amount conversion and preferably mass percent 1 ～10%, more preferably mass percent 2～10%, more preferably mass percent 3～10%.When the content of Sn is in institute When in the range of stating, target has low-resistance advantage.
In the case where ceramics are for AZO, the content of the Al in the target is with Al2O3Amount conversion and preferably mass percent 0.1～5%, more preferably mass percent 1～5%, more preferably mass percent 2～5%.When the content of Al is in institute When in the range of stating, target has low-resistance advantage.
In the case where ceramics are for IGZO, preferably, the content of the In in the target is with In2O3Amount is scaled quality percentage Content than 40～60%, Ga is with Ga2O3Amount is scaled mass percent 20～50%, and the content of Zn is scaled quality with ZnO amounts Percentage ratio 5～30%, more preferably, the content of In is with In2O3Amount is scaled mass percent 40～55%, the content of Ga with Ga2O3Amount is scaled mass percent 25～35%, and the content of Zn is scaled mass percent 15～30% with ZnO amounts, further Preferably, the content of In is with In2O3Amount is scaled mass percent 40～50%, and the content of Ga is with Ga203Amount is scaled quality hundred The content of ratio 25～35%, Zn is divided to be scaled mass percent 20～30% with ZnO amounts.When the content of In, Ga and Zn is in institute When in the range of stating, with good TFT (thin film transistor (TFT)s are obtained by sputtering：Thin Film Transistor) characteristic Advantage.
<Ceramic cylindrical sputtering target>
The ceramic cylindrical sputtering target of the present invention is, by grafting material by the ceramic cylindrical sputtering target material and backing Pipe joint and formed.
The backing Gutron often has the drum that can be engaged ceramic cylindrical sputtering target material.Species to backing pipe Especially do not limit, can suitably be selected to use according to target from existing used backing pipe.For example, make For the material of backing pipe, rustless steel, titanium etc. can be included.
The species of the grafting material is also not particularly limited, can be according to target from existing used jointing material In suitably selected to use.For example, as jointing material, solder of indium etc. can be included.
A piece engageable outside in a backing pipe of ceramic cylindrical sputtering target material, it is also possible to by more than two side by side Ground engagement is on the same axis.In the case that more than two are abreast engaged, gap between each ceramic cylindrical target, I.e. the length of cutting part is usually 0.05～0.5mm, more preferably preferably 0.05～0.3mm, 0.05mm.Although cutting part During length shorter sputtering, electric arc is less susceptible to produce, but when less than 0.05mm, it is possible to because in engaging process, sputter procedure In thermal expansion, and make target it is impinging one another, rupture.
Joint method is not particularly limited, can using with existing ceramic cylindrical sputtering target material identical method.
<The manufacture method of ceramic cylindrical target>
The manufacture method of the ceramic cylindrical sputtering target material of the present invention, including：Operation 1, by containing ceramic material powder with And the serosity of organic additive is preparing granule；Operation 2, CIP molding is carried out to the granule so as to produce it is columnar into Type body；Operation 3, carries out defat to the molded body；And operation 4, the molded body of the defat is sintered, the ceramics The manufacture method of tubular sputtering target material is characterised by, in the operation 1, the amount of the organic additive is relative to described The amount of ceramic material powder is mass percent 0.1～1%.
By this manufacture method, the ceramic cylindrical sputtering target material that can effectively manufacture the present invention that sends as an envoy to is not produced Crackle, deformation.
In the manufacture method, preferably, the organic additive contains binding agent, the binding agent be polyvinyl alcohol, institute The degree of polymerization for stating polyvinyl alcohol is 200～400 and basicity molar percentage is 60～80%.
(operation 1)
In operation 1, granule is prepared by the serosity containing ceramic material powder and organic additive.
Granule is prepared by by ceramic material powder and organic additive, and the granule is supplied to the CIP of operation 2 Molding such that it is able to obtain making the fillibility of raw material to improve and highdensity molded body.Additionally, filling inequality is not susceptible to and can It is uniform to fill.Punching press inequality is also less likely to occur.
Ceramic material powder is the powder of the ceramics that the structural material as target can be produced by the manufacture method End.
For example, in the case where ceramics are for ITO, as ceramic material powder, In can be used2O3Powder and SnO2Powder Mixed-powder, can be used alone ito powder, or and In2O3Powder and SnO2Powder is used in mixed way.Using BET (Brunauer-Emmett-Teller) method is determining In2O3Powder, SnO2The specific surface area of powder and ito powder is generally divided Wei not 1～40m2/g。In2O3Powder, SnO2The blending ratio of powder and ito powder is contained with the constitution element in the target Measure the mode in described scope and be appropriately determin.In the manufacture method, by In2O3Powder and SnO2Powder In the case that mixed-powder carrys out use as ceramic material powder, the SnO in ceramic material powder is confirmed2The content of powder (mass percent %) can be regarded as, with the SnO in finally obtained target2Content (the quality percentage of the Sn of amount conversion Than %).
In the case where ceramics are for AZO, as ceramic material powder, Al can be used2O3The mixing of powder and ZnO powder Powder, can be used alone AZO powder, or and Al2O3Powder and ZnO powder are used in mixed way.Determined using BET method Al2O3The specific surface area of powder, ZnO powder and AZO powder typically respectively 1～40m2/g。Al2O3Powder, ZnO powder and The blending ratio of AZO powder is properly determined in the way of the content of structural element in the target is in the scope.At this In manufacture method, by Al2O3In the case that the mixed-powder of powder and ZnO powder carrys out use as ceramic material powder, confirm The Al gone out in ceramic material powder2O3The content (mass percent %) of powder is regarded as, with finally obtained target in Al2O3The content (mass percent %) of the Al of amount conversion.
In the case where ceramics are for IGZO, as ceramic material powder, In can be used2O3Powder, Ga2O3Powder and ZnO The mixed-powder of powder, can be used alone IGZO powder, or and In2O3Powder, Ga2O3Powder and ZnO powder mixing make With.In is determined using BET method2O3Powder, Ga2O3The specific surface area of powder, ZnO powder and IGZO powder typically respectively 1 ～40m2/g。In2O3Powder, Ga2O3The blending ratio of powder, ZnO powder and IGZO powder is contained with structural element in the target Measure the mode in the scope and be properly determined.In the manufacture method, by In2O3Powder, Ga2O3Powder and ZnO powder In the case that the mixed-powder at end carrys out use as ceramic material powder, the In in ceramic material powder is confirmed2O3Powder, Ga2O3The content (mass percent %) of powder and ZnO powder is regarded as respectively, with finally obtained target in In2O3 Amount conversion In content (mass percent %), with Ga2O3The content (%) of the Ga of amount conversion and the Zn with ZnO amount conversions Content (mass percent %).
Obtained from using the mixing different two or more powder of particle diameter during ceramic material powder, due to particle diameter it is larger Powder granule between doped with the less powder of particle diameter granule, therefore the density with formed body uprises, sintered body it is strong Spend enhanced advantage.
The mixed method of powder is not particularly limited, for example, each powder and zirconium oxide spheroid cylinder can be inserted In body, ball mill mixing is carried out.
The organic additive is, adjusts serosity, the character of formed body and the material that adds for appropriate.Add as organic Plus thing, binding agent, dispersant and plasticizer etc. can be included.
In operation 1, the amount of organic additive is mass percent 0.1～1.2% relative to the amount of ceramic material powder, Preferably mass percent 0.2～1.0%, more preferably mass percent 0.4～0.8%.Described when organic additive mixes When resultant is more than mass percent 1.2%, it sometimes appear that the intensity decreases degree of the molded body in skimming processes become it is big and The situation of defat cracking is produced easily, it sometimes appear that the emptying aperture in defat aftershaping body increases so as to be difficult to densification Situation.When the combined amount of organic additive is less than mass percent 0.1%, has sometimes and cannot obtain each composition Sufficient effect.When the combined amount by organic additive sets within the above range, length can be produced for more than 500mm And relative density is more than the 95% ceramic cylindrical sputtering target material as integrated component.
Binding agent is, for the ceramic material powder in molded body is bonded, to add so as to improve the intensity of molded body Plus.As binding agent, when obtaining molded body in being usable in known powder sintering and commonly used binding agent.
Wherein, preferably polyvinyl alcohol (PVA), and being preferably, the degree of polymerization is 200～400 and basicity is moles hundred Divide the polyvinyl alcohol than 60～80%.When using such binding agent, even if the addition of binding agent is a small amount of, also can be The granule being easily deformed is prepared during CIP molding, densely being not easy filled with ceramic material powder is obtained by CIP molding The molded body of cracking, its result is, it is possible to produce will not make the ceramic cylinder of crackle, the high density that deformation is produced and long size Shape target.For example, when the combined amount by organic additive sets within the above range, and during using described adhesive, Ke Yiwen Surely length is produced for more than 750mm, the ceramic cylindrical target of the integrated component that relative density is more than 95%.
Generally, when by the operation of molding, defat and sintering, ceramic powders are fabricated to into the pottery of longer size During porcelain cylindrical shape target, crackle can be produced in any operation of molding, defat and sintering.Therefore, in existing manufacturer In method, it is impossible to produce length for more than 500mm, the ceramic cylindrical target of the integrated component that relative density is more than 95%. When in CIP molded bodys, crackle during molding become growth size, it is large-scale when, it is believed that crackle during molding is due to resilience Power becomes big and causes.In the case of cast molding body, it is believed that because moisture is uneven, microgranule segregation is ftractureed for starting point.Though As long as so increasing the situation that amount of binder can then eliminate molding crackle, but when amount of binder is increased, in defat or burnt till In journey, cylinder molded body is brittle and rupture.Further, since the excessive binding agent of addition can become binding agent segregation and defat cracking Starting point, so not preferred.
In the manufacture method of the present invention, by using described adhesive, even if the molded body of long size, also can be by adding Plus a small amount of binding agent and obtain the molded body being not easily susceptible to cracking, therefore cylinder molded body is difficult in defat and sintering process Rupture.That is, when using described adhesive, it is not easy to crack in molding, defat and any operation in burning till, can The ceramic cylindrical target of long size is obtained stably.
It is believed that by using described adhesive, it is based on following reason that can obtain such effect.
For example, by the serosity containing material powder, binding agent and water by being spray-dried preparing the feelings of granule Under condition, outer side shifting of the water to drop is made by being dried in the drop sprayed to serosity and formed, at the same time make original Feed powder end and binding agent are also to the outer side shifting of drop.Water is volatilized outside drop, and its result is, material powder and viscous Mixture densely coagulation in droplet surface portion, and form the granule with hard envelope.Due to material powder, binding agent with And water is moved in peripheral part and makes the granule be changed into hollow, therefore the hollow bulb is negative pressure.In order to eliminate the pressure differential and Granule is made to be recessed.As the granule of such depression is harder, therefore it is unlikely to deform in molding.Therefore, molded body can be produced not Densification, and the big defect of the starting point of cracking can be become., it can be said that such situation is to produce when the molded body of long size is made The main cause of the situation of raw cracking.
When using the degree of polymerization that the degree of polymerization is 200～400 relatively low binding agent, the composition as binding agent is obtained in that High molecular complexation it is less, and the relatively low serosity of viscosity.When using by binding agent, than being set to, the fixed and degree of polymerization is relatively low to glue During mixture, the high serosity of material powder concentration can be produced with low viscosity.Therefore, because when serosity is sprayed in drop The movement of water is less, therefore is difficult to form hollow inside granule, and is difficult to be recessed.Due to the binding agent in granule complexation compared with It is few, therefore the adhesion of binding agent is weaker, so as to granule is easily deformed.Additionally, when the serosity of high concentration is sprayed, by Coagulation is unable in the surface element of drop in material powder and binding agent, therefore surface element is difficult to become fine and close, so that granule Intensity step-down.According to the reasons why such, it is believed that can be obtained by CIP molding and be densely filled with ceramic material powder Easily rupturable molded body is not allowed.
Additionally, when using the basicity that basicity is molar percentage 60～80% relatively low binding agent, by raw material Powder, binding agent and water and in the serosity that formed, the hydrophobic group of binding agent adsorbs on powder, so as to obtain dispersibility Higher serosity.When sprayed by serosity, binding agent is separated out at short notice, and not to The outer side shifting of drop, thus on whole granule it is dispersed have binding agent in the state of be dried, it is hereby achieved that table The relatively low granule of facial intensity.According to the reasons why such, it is believed that can obtain densely former filled with ceramics by CIP molding The molded body at feed powder end.
As mentioned above, although be a less side as the degree of polymerization and basicity of the polyvinyl alcohol of binding agent, can To obtain yielding granule.It is therefore preferable that be, as binding agent polyvinyl alcohol the degree of polymerization below 400, basicity is Below molar percentage 80%.On the other hand, when the degree of polymerization and too small basicity, the molded body for being obtained will become excessively Soft and operability will decline.It is therefore preferable that be, as binding agent polyvinyl alcohol the degree of polymerization more than 200, basicity is Molar percentage more than 60%.More preferably, the degree of polymerization as the polyvinyl alcohol of binding agent be molar percentage 250～ 350%, basicity is molar percentage 65～75%, and more preferably, the degree of polymerization is molar percentage 280～320, is alkalized Spend for molar percentage 68～72%.
As binding agent polyvinyl alcohol addition relative to ceramic material powder preferably mass percent 0.1～ 1.0%, more preferably mass percent 0.1～0.65%, more preferably mass percent 0.1～0.3%.Polyvinyl alcohol Addition it is more, the higher molding of plasticity more becomes to be not easily susceptible to cracking, and it sometimes appear that molded body in skimming processes Intensity decreases degree become greatly and easily produce defat ftracture situation, it sometimes appear that defat aftershaping body hollow hole increase so as to Become to be not easy to the situation of densification.Therefore, the scope is preferred.
Dispersant is to add for improving the dispersibility of the material powder in serosity and binding agent.As dispersion Agent, can include, for example polycarboxylic acids ammonium, ammonium polyacrylate etc..
Plasticizer is to add for improving the plasticity of molded body.As plasticizer, can include, for example, gather Ethylene glycol (PRG), ethylene glycol (EG) etc..
The disperse medium used when the serosity containing ceramic material powder and organic additive is prepared is without especially Limit, can properly select to use from water, ethanol etc. according to purpose.
It is not particularly limited in the method containing ceramic material powder and the serosity of organic additive of preparation, example Such as, it is possible to use ceramic material powder, organic additive and disperse medium are put in tank, carry out the side of ball mill mixing Method.
It is not particularly limited in the method that granule is prepared by serosity, for example, spray drying method, rotation can be used to make Grain method, extruder grain method etc..Wherein, it is higher in the mobility of granule, the side of easily deformable granule is easily produced during molding Face, preferably spray drying method.For the condition of spray drying method is not particularly limited, Ceramic Material powder can be suitably selected In the pelletize at end, commonly used condition is implementing.
(operation 2)
In operation 2, the granule prepared by operation 1 is carried out into CIP molding (Cold Isostatic Pressing (cold isostatic compaction)) and produce columnar molded body.When molded body is produced by CIP molding, it is possible to obtain Density is homogeneous and directivity is less, even if implementing defat and burning till the columnar molded body of long size for being not easy to ftracture.
As the model used in CIP molding, size circle being usually used in CIP molding, long can be produced The model of the molded body of tubular, it is, for example possible to use having the poly- of up and down sealable lid and columned core (heart axle) Urethane rubber etc..
Pressure during CIP molding is usually 800kgf/cm2More than, preferably 1000kgf/cm2More than, more preferably 3000kgf/cm2More than.Pressure is bigger, more can densely filler particles such that it is able to make molded body densification and high-strength Degreeization.For upper limit of pressure value during CIP molding is not particularly limited, usually 5000kgf/cm2。
When being reduced pressure after being pressurizeed in CIP forming processes, pressure is in 200kgf/cm2It is in following scope, excellent Decompression rate is set to 200kgf/cm by choosing2Decompression rate is more preferably set to 100kgf/cm by below h2Below h, further It is preferred that decompression rate is set to 50kgf/cm2Below h.Due in 200kgf/cm2In decompression in following scope, molded body The resilience force of upper generation is stronger, therefore molded body is easily broken.When decompression rate is set to 200kgf/cm2During below h, return Elastic force dies down, and molded body is not easily broken.When with such decompression rate implement reduce pressure when, stably can produce high density and The ceramic cylindrical target of long size.For example, when described adhesive is used, the combined amount of organic additive is located at into the scope It is interior, and during using the decompression rate, can stably produce length for more than 1000mm and relative density is more than 95% Integrated component ceramic cylindrical target.The lower limit of decompression rate is not particularly limited, usually 30kgf/cm2。
It is higher than 200kgf/cm to pressure2In the range of decompression rate be not particularly limited, usually 200～ 1000kgf/cm2·h。
(operation 3)
In operation 3, the molded body to being produced by operation 2 carries out defat.Defat is by heating to molded body And implement.
Skimming temp is usually 600～800 DEG C, preferably 700～800 DEG C, more preferably 750～800 DEG C.Although defat The intensity of the higher molded body of temperature is higher, but as the contraction of molded body when more than 800 DEG C, can be caused, therefore be preferably Defat is carried out below 800 DEG C.
Degreasing time is usually 3～10 hours, preferably 5～10 hours, more preferably 10 hours.Although degreasing time is got over The intensity of long molded body is higher, but due to being substantially completed defat by the heating of 10 hours, even if therefore by degreasing time It is set to also improve more than the intensity of 10 hour molded bodys.
Programming rate is being reached within the temperature range of 400 DEG C, preferably 50 DEG C/below h, more preferably 30 DEG C/below h, More preferably 20 DEG C/below h.Defat is carried out till reaching 400 DEG C due to working as, and is carried out in skimming processes high speed During intensification, molded body becomes prone to rupture, therefore is preferably, and is heated up with the low speed of 50 DEG C/below h till reaching 400 DEG C. When will heat up speed and being located in the scope, can be stably producing the ceramic cylindrical target of high density and long size Material.For example, when described adhesive is used, the combined amount of organic additive is located in the scope, and by subtracting during CIP molding Pressure speed is located in the scope, and when programming rate during defat is located at the scope, can stably produce length Spend the ceramic cylindrical target of the integrated component for more than 1500mm and relative density more than 95%.Due to higher than 400 DEG C with On temperature in defat complete, therefore in order to shorten process time, can at faster speed, for example 50 DEG C/h or so is carried out Heat up.
(operation 4)
In operation 4, to being sintered by the molded body of defat in operation 3.
Calcining furnace is not particularly limited, existing used calcining furnace in the manufacture of ceramic target is usable in.
In the case where ceramics are for ITO, sintering temperature is usually 1450～1700 DEG C, preferably 1500～1650 DEG C, more Preferably 1550～1600 DEG C.In the case where ceramics are for AZO or IGZO, usually 1250～1500 DEG C, preferably 1300～ 1450 DEG C, more preferably 1350～1400 DEG C.Although sintering temperature is more high more can obtain highdensity target, when too high When, the sintering structure hypertrophyization of target will be made and become to be easily broken.
Sintering time is usually 3～30 hours, preferably 5～10 hours, more preferably 5～8 hours.Although sintering time The easier densification of longer target, but when long, the sintering structure hypertrophyization of target will be made and become to be easily broken.
Programming rate is usually 100～500 DEG C/h.Cooling rate be usually 10～100 DEG C/h, preferably 10～50 DEG C/ H, more preferably 10～30 DEG C/h.Although cooling rate is less to be less susceptible to produce the crackle because caused by thermal stress difference, i.e., Make to be set to poor less than 10 DEG C/h thermal stress will not generally also change.
It is not particularly limited to calcining atmosphere, usually atmospheric atmosphere or oxygen atmosphere.
The sintered body for being obtained is used by implementing the necessary processing such as machining to be used as sputtering target material.
Embodiment
The evaluation methodology of the sputtering target material obtained in embodiment and comparative example is as described below.
1. relative density
The relative density of sputtering target material is determined based on Archimedes method.Specifically, by the aerial of sputtering target material Weight divided by volume (the water proportion in the water of=sputtering target sintered body in weight/measurement temperature), and relative to based on following numbers The value of the percentage rate of the solid density ρ (g/cm3) of formula (X) is set to relative density.(unit：%).
[mathematical expression 1]
(in mathematics formula (X), C1～CiThe content (percentage by weight %) of the structural material of target, ρ are represented respectively1～ρi Represent and C1～CiDensity (the g/cm of each corresponding structural material3))。
2. the evaluation of the cracking of sputtering target material or molded body
Sputtering target material and molded body are observed by visual observation, it is unconfirmed crackle occur on sputtering target material or molded body In the case of be evaluated as " A ", " B " is evaluated as in the case of confirming.
＜ ITO target ＞
[embodiment 1]
It is 10m by the specific surface area measured by BET method2The SnO of/g2Powder and the ratio measured by BET method Surface area is 10m2The In of/g2O3Powder is so that SnO2Amount become the mode of mass percent 1% and mixed, and in tank Ball mill mixing is carried out by zirconia ball, so as to prepare ceramic material powder.
In the tank, as binding agent, for ceramic material powder adds the polyvinyl alcohol of mass percent 0.1% (poly- It is right：280, basicity be molar percentage 68%), as dispersant, for ceramic material powder adds mass percent 0.3% polycarboxylic acids ammonium, and as disperse medium, for ceramic material powder adds the water of mass percent 15%, carry out Ball mill mixes and prepares serosity.Total amount (total amount of polyvinyl alcohol amount and polycarboxylic acids ammonium amount) relative to organic additive The ratio of the amount of ceramic material powder is mass percent 0.4%.
The serosity is supplied into spray-drying installation, is 10000rpm in atomization rotating speed, inlet temperature is 250 DEG C of bar Implement spray drying to prepare granule under part.
Rap the granule while being filled in sealable lid up and down and with the cylindric of external diameter 165mm Core (heart axle) internal diameter be 210mm (wall thickness is 10mm), length for 1219mm drum polyurethane rubber model In, and will be rubber cast closed after, with 800kgf/cm2Pressure carry out CIP molding, so as to produce columnar molding Body.Decompression rate after CIP molding is higher than 200kgf/cm2Pressure limit in be set to 300kgf/cm2H, is being less than 200kgf/cm2In the range of be set to 200kgf/cm2·h.The length of the molded body for being obtained is 1212mm.
Heating defat is carried out to the molded body.Skimming temp is 700 DEG C, and degreasing time is 10 hours, and programming rate is reaching 20 DEG C/h is set to in the range of 400 DEG C, 50 DEG C/h is set in the range of higher than 400 DEG C.
The molded body of defat is sintered, so as to produce sintered body.It is sintered to, in atmospheric atmosphere, sintering temperature 1600 DEG C are set to, sintering time is set to 10 hours, programming rate is set to 300 DEG C/h, and cooling rate is set to 50 DEG C/h.
Sintered body to being obtained carries out machining, and so as to produce external diameter for 155mm, internal diameter is 135mm, and length is The ITO tubular sputtering target materials of 1000mm.
It is 133mm that three targets are passed through In solder bonds in external diameter, and internal diameter is 123mm, and length is 3200mm's On SUS304 backing pipes, so as to produce ITO targets.Interval (length of cutting part) between each target is set to 0.2mm.
Relative density of the table 1 for expression target, and the evaluation of the crackle of target and molded 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 powder2The content of powder, the degree of polymerization of polyvinyl alcohol and basicity and polyethylene The addition of alcohol, the addition of polycarboxylic acids ammonium are set to the condition shown in table 1, in addition the reality in the way of similarly to Example 1 Apply, so as to prepare granule.
CIP molding is carried out to the granule, so as to produce the columnar molded body with the length shown in table 1.In CIP In molding, embodiment 2,3,9～18, comparative example 6 uses polyurethane rubber model same as Example 1, and is related to other Embodiment and comparative example, using with the polyurethane rubber model identical core and internal diameter used in embodiment 1, And the polyurethane rubber type of the length with the molded body that can obtain length as shown in table 1.After by CIP molding, 200kgf/ cm2Decompression rate in the range of pressures below is set to the condition shown in table 1.CIP conditions of molding in addition and 1 phase of embodiment Together.In comparative example 5, crackle is generated on molded body in molding procedure.
Molded body to not cracking in molding procedure carries out heating defat.It is up within the temperature range of 400 DEG C Programming rate be set to the condition shown in table 1, degreasing condition in addition is same as Example 1.In comparative example 1～4 and 8 In～9, crackle is generated on molded body in degreasing process.
What is do not cracked in degreasing process with condition same as Example 1 is burnt by the molded body of defat Knot, so as to produce sintered body.Sintered body to being obtained carries out machining, so as to produce with the external diameter shown in table 1, The ITO tubular sputtering target materials of internal diameter and length.
In order to obtain the quantity of the cutting part shown in table 1, and pass through In solders by many (more than the quantity one of cutting part Radical) the target be bonded on external diameter for 133mm, internal diameter is 123mm, SUS304 backing pipe of the length for 3200mm On, so as to produce ITO target.Interval (length of cutting part) between each target is set to 0.2mm.
The evaluation of the crackle of the relative density and target and molded body of each target that table 1 is obtained by expression.
＜ AZO target ＞
[embodiment 21]
It is 5m by the specific surface area measured by BET method2The Al of/g2O3Powder and the ratio measured by BET method Surface area is 10m2The ZnO powder of/g is so that Al2O3Content become the mode of mass percent 0.5% and mixed, and in tank In ball mill mixing is carried out by zirconia ball, so as to prepare ceramic material powder.
In addition to using the ceramic material powder, implement in the way of similarly to Example 1, prepare granule.
Under the same conditions as example 1, using with sealable lid up and down and with the cylinder that external diameter is 167mm The polyurethane rubber model of the drum that the internal diameter of the core (heart axle) of shape is 213mm (wall thickness 10mm), length is 1233mm, CIP molding is carried out to the granule, so as to produce the columnar molded body with the length shown in table 2.
Defat is carried out to the molded body under the same conditions as example 1.
Under the same conditions as example 1 to being sintered by the molded body of defat, so as to produce sintered body.To institute The sintered body machining of acquisition, so as to produce the sputtering of the AZO cylindrical shapes with the external diameter shown in table 2, internal diameter and length Target.
It is 133mm that three targets are passed through In solder bonds in external diameter, and internal diameter is 123mm, and length is 3200mm's On SUS304 backing pipes, so as to produce AZO targets.Interval (length of cutting part) between each target is set to 0.2mm.
Evaluation of the table 2 for the crackle of the relative density and target and molded body of expression target.
[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 powder2O3The content of powder, the degree of polymerization of polyvinyl alcohol and basicity, and polyethylene The addition of the addition and polycarboxylic acids ammonium of alcohol is set to the condition of the expression of table 2, in addition with side similarly to Example 21 Formula is implemented, so as to prepare granule.
CIP molding is carried out to the granule, so as to produce the cylindrical shape molded body with length shown in table 2.In CIP molding In, during embodiment 22,28～30,33, comparative example 14, use and 21 identical polyurethane rubber of embodiment, be related to Other embodiments and comparative example, using with the polyurethane rubber identical core used in embodiment 21 and interior Footpath, and the polyurethane rubber of the length with the molded body that can obtain length as shown in table 2.After by CIP molding, 200kgf/cm2Decompression rate in the range of pressures below is set to the condition shown in table 2.The condition of CIP molding in addition sets It is identical with embodiment 21.In comparative example 13, crackle is generated on molded body in molding procedure.
Molded body to not cracking in molding procedure carries out heating de- ester.It is up within the temperature range of 400 DEG C Programming rate is set to condition shown in table 2, and degreasing condition in addition is set to identical with embodiment 21.In comparative example 10～12 And in 16～18, crackle is generated on molded body in degreasing process.
With with 21 identical of embodiment under the conditions of to being burnt by the molded body of defat for slight crack is not produced in degreasing process Knot, so as to produce sintered body.Machining is carried out to resulting sintered body, so as to produce with the external diameter shown in table 2, The AZO tubular sputtering target materials of internal diameter and length.
In order to obtain the quantity of cutting part shown in table 2, and pass through In solders and (be more than the quantity one of cutting part by many Radical) target is bonded on external diameter for 133mm, internal diameter is 123mm, length on the SUS304 backing pipes of 3200mm, from And produce AZO targets.Interval (length of cutting part) between each target is set to 0.2mm.
The relative density of each target that table 2 is obtained by expression, and the evaluation of the crackle of target and molded body.
＜ IGZO target ＞
[embodiment 34]
It is 10m by the specific surface area measured by BET method2The In of/g2O3Powder and measured by BET method Specific surface area is 10m2The Ga of/g2O3Powder and the specific surface area measured by BET method are 10m2The ZnO powder of/g so that In2O3The content of powder becomes mass percent 44.2%, Ga2O3The content of powder be mass percent 29.9%, ZnO powder Content mixed for the mode of mass percent 25.9%, and ball mill mixing is carried out by zirconia ball in tank, from And prepare ceramic material powder.
Except using the ceramic material powder, and replace the polyvinyl alcohol (degree of polymerization：280, basicity side's molar percentage 68%) use the polyvinyl alcohol (degree of polymerization：500, basicity be molar percentage 90%) beyond, according to same as Example 1 Mode implement, so as to prepare granule.
Using the internal diameter with up and down sealable lid and with external diameter for the columned core (heart axle) of 171mm it is The polyurethane rubber of 218mm (heavy wall), length for the drum of 653mm, except after by CIP molding, 200kgf/cm2With Under pressure limit in decompression rate be set to 300kgf/cm2Beyond h, under the same conditions as example 1 to the granule CIP molding is carried out, so as to produce the columnar molded body with length shown in table 3.
Defat is carried out to the molded body under the same conditions as example 1.
Under the same conditions as example 1 to being sintered by the molded body of defat, so as to produce sintered body.To institute The sintered body for obtaining carries out machining, so as to produce the IGZO cylindrical shapes with the external diameter shown in table 3, internal diameter and length Sputtering target material.
It is 133mm that target described in the six roots of sensation is bonded on external diameter by In solders, and internal diameter is 123mm, and length is 3200mm's On SUS304 backing pipes, so as to produce IGZO targets.Interval (length of cutting part) between each target is set to 0.2mm.
Relative density of the table 3 for expression target, and the evaluation of the crackle of target and molded 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 powder2O3The content of powder, Ga2O3It is the content of the content and ZnO powder of powder, poly- The degree of polymerization and basicity of vinyl alcohol, and the addition of the addition and polycarboxylic acids ammonium of polyvinyl alcohol is set to the bar shown in table 3 Part, in addition the mode same with embodiment 34 implement, so as to prepare granule.
CIP molding is carried out to the granule, so as to produce the cylindrical shape molded body with length shown in table 3.In CIP molding In, during embodiment 35～36, comparative example 19～20,22～25, use and 34 identical polyurethane rubber of embodiment, and Be related to other embodiments and comparative example, using with the polyurethane rubber identical core used in embodiment 34 And internal diameter, and the polyurethane rubber of the length with the molded body that can obtain length as shown in table 2.After CIP molding , 200kgf/cm2Decompression rate in the range of pressure below is set to condition shown in table 3.The bar of CIP molding in addition Part is set to identical with embodiment 34.In comparative example 20, crackle is generated on molded body in molding procedure.
Molded body to slight crack is not produced in molding procedure carries out heating defat.It is up within the temperature range of 400 DEG C Programming rate is set to the condition shown in table 3, and degreasing condition in addition is set to identical with embodiment 34.In comparative example 19 and In 23～25, crackle is generated on molded body in degreasing process.
Under the conditions of with 34 identical of embodiment to degreasing process in do not produce being burnt by the molded body of defat for slight crack Knot, so as to produce sintered body.Resulting sintered body is carried out into machining, so as to produce with the external diameter shown in table 3, The IGZO tubular sputtering target materials of internal diameter and length.
In order to obtain the quantity of cutting part shown in table 3, by In solders by many (more than one of quantity of cutting part Radical) target is bonded on external diameter for 133mm, internal diameter is 123mm, length on the SUS304 backing pipes of 3000mm, from And produce IGZO targets.Interval (length of cutting part) between each target is set to 0.2mm.
The relative density of each target that table 3 is obtained by expression, and the evaluation of the crackle of target and molded body.
As shown in table 1～3, it is obtained in that in the embodiment 1～44 of manufacture method of the present invention is implemented a kind of as follows Target, i.e. the crackle of target and molded body is not produced in the manufacturing process of target, the length with more than 500mm and is had The ITO tubular sputtering target materials of more than 95% relative density, AZO tubular sputtering targets material or IGZO tubular sputtering targets material with And the target formed by these.
In enforcement is not the comparative example of manufacture method of the invention, the amount of organic additive is relative to ceramic material powder Amount and in the case of being more than mass percent 1.2%, crack on molded body in degreasing process, or the phase of target Density is less than in the case of 95%, is cracked on molded body in molding procedure.In a comparative example, it is impossible to which manufacture is provided There are the length and the ceramic cylindrical sputtering target material with more than 95% relative density of more than 500mm.

Claims (8)

1. a kind of ceramic cylindrical sputtering target material, it is characterised in that
The ceramic cylindrical sputtering target material is, length be more than 750mm and relative density be more than 99% integrated component Sintered body.
2. ceramic cylindrical sputtering target material as claimed in claim 1, it is characterised in that
The length of the ceramic cylindrical sputtering target material is more than 1000mm.
3. ceramic cylindrical sputtering target material as claimed in claim 1, it is characterised in that
The length of the ceramic cylindrical sputtering target material is more than 1500mm.
4. the ceramic cylindrical sputtering target material as described in any one in claims 1 to 3, it is characterised in that
Described ceramic cylindrical sputtering target material is the content of Sn with SnO2Amount is scaled the Indium sesquioxide. of mass percent 1～10% Stannum system.
5. the ceramic cylindrical sputtering target material as described in any one in claims 1 to 3, it is characterised in that
Described ceramic cylindrical sputtering target material is the content of Al with Al2O3Amount is scaled the aluminum of mass percent 0.1～5% and mixes Miscellaneous Zinc Oxide system.
6. the ceramic cylindrical sputtering target material as described in any one in claims 1 to 3, it is characterised in that
Described ceramic cylindrical sputtering target material is the content of In with In2O3Amount is scaled mass percent 40～60%, and Ga's contains Amount is with Ga2O3Amount is scaled mass percent 20～40%, and the content of Zn is scaled mass percent 10～30% with ZnO amounts Indium gallium zinc oxide system.
7. a kind of ceramic cylindrical sputtering target material, it is characterised in that
The tubular sputtering target material described in any one in claims 1 to 3 is engaged on backing pipe by grafting material and Formed.
8. a kind of manufacture method of ceramic cylindrical sputtering target material, wherein, the ceramic cylindrical sputtering target material is claim 1 Ceramic cylindrical sputtering target material in～6 described in any one,
The manufacture method of the ceramic cylindrical sputtering target material includes：
Operation 1, prepares granule by the serosity containing ceramic material powder and organic additive；
Operation 2, carries out CIP molding so as to produce columnar molded body to the granule；
Operation 3, carries out defat to the molded body；And
Operation 4, is sintered to the molded body of the defat,
The manufacture method of the ceramic cylindrical sputtering target material is characterised by,
In the operation 1, the amount of the organic additive is mass percent 0.1 relative to the amount of the ceramic material powder ～0.6%,
The organic additive contains binding agent, and the binding agent is that the degree of polymerization is 200～400 and basicity is molar percentage 60～80% polyvinyl alcohol.
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