JPH11228219A - Production of high-density ito sintered compact utilizing ito recycled powder - Google Patents
Production of high-density ito sintered compact utilizing ito recycled powderInfo
- Publication number
- JPH11228219A JPH11228219A JP10027055A JP2705598A JPH11228219A JP H11228219 A JPH11228219 A JP H11228219A JP 10027055 A JP10027055 A JP 10027055A JP 2705598 A JP2705598 A JP 2705598A JP H11228219 A JPH11228219 A JP H11228219A
- Authority
- JP
- Japan
- Prior art keywords
- ito
- powder
- density
- sintered body
- recycled
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、スパッタリング法
で透明導電膜を形成する際に用いられるスパッタリング
ターゲットとして用いるに好適な高密度ＩＴＯ焼結体の
製造方法に関する。The present invention relates to a method for manufacturing a high-density ITO sintered body suitable for use as a sputtering target used when forming a transparent conductive film by a sputtering method.
【０００２】[0002]
【従来の技術】酸化インジウム−酸化錫（Ｉｎ2 Ｏ3 −
ＳｎＯ2 、以下、「ＩＴＯ」という）膜は、可視光透過
性が高く、かつ導電性が高いので透明導電膜として液晶
表示装置やガラスの結露防止用発熱膜等に幅広く用いら
れている。このＩＴＯ膜の形成方法としては、ＩＴＯ焼
結体をスパッタリング用ターゲットとして用いる方法が
広く行われている。スパッタリング法におけるターゲッ
トの利用効率は２０〜４０重量％程度であり、残りの使
用済みターゲットは廃棄処分または再生工程を経て、再
び原料として酸化インジウム粉を製造していた。 2. Description of the Related Art Indium oxide-tin oxide (In 2 O 3 −
The SnO 2 (hereinafter referred to as “ITO”) film has a high visible light transmittance and a high conductivity, and is therefore widely used as a transparent conductive film for a liquid crystal display device, a heat generation film for preventing dew condensation on glass, and the like. As a method for forming the ITO film, a method using an ITO sintered body as a sputtering target is widely used. The use efficiency of the target in the sputtering method is about 20 to 40% by weight, and the remaining used target has been subjected to a disposal process or a regeneration process to produce indium oxide powder again as a raw material.
【０００３】特開平７−３１６７９８号公報には、使用
済みＩＴＯターゲットを洗浄後、自生粉砕によって粉末
とし（以下「ＩＴＯリサイクル粉」という）、この粉末
をホットプレス法などによって焼結体とする方法が記載
されている。この方法を用いれば使用済みＩＴＯターゲ
ットを、酸化インジウム粉に再生せずにＩＴＯ焼結体を
得ることができるが、密度が９０％（６．４８ｇ／ｃｍ
3 ）程度であり、さらに高密度化することは困難であっ
た。ここでＩＴＯ焼結体に高密度化が要求される理由
は、スパッタリング時の成膜条件やＩＴＯ膜質の諸特性
が優れているためである。[0003] Japanese Patent Application Laid-Open No. Hei 7-316798 discloses a method in which a used ITO target is washed and then powdered by autogenous pulverization (hereinafter referred to as "ITO recycled powder"), and this powder is formed into a sintered body by hot pressing or the like. Is described. By using this method, it is possible to obtain an ITO sintered body without regenerating a used ITO target into indium oxide powder, but the density is 90% (6.48 g / cm).
3 ) and it was difficult to further increase the density. The reason why the ITO sintered body is required to have a higher density is that the film forming conditions during sputtering and various properties of the ITO film are excellent.
【０００４】[0004]
【発明が解決しようとする課題】本発明の目的は、ＩＴ
Ｏリサイクル粉を原料とした泥漿鋳込み成形法により、
スパッタリングターゲットとして用いるに好適な高密度
のＩＴＯ焼結体の製造方法を提供することにある。SUMMARY OF THE INVENTION The object of the present invention is to provide an IT
By a slurry casting method using O recycled powder as a raw material,
An object of the present invention is to provide a method for producing a high-density ITO sintered body suitable for use as a sputtering target.
【０００５】[0005]
【課題を解決するための手段】本発明者らは、ＩＴＯリ
サイクル粉を利用して高密度のＩＴＯ焼結体を製造する
ために、ＩＴＯリサイクル粉を熱処理し、比表面積を
２．５〜７．０ｍ2 ／ｇの範囲に調整した粉末を用いて
泥漿鋳込み成形法によって成形し、得られた成形体を乾
燥後、酸素雰囲気で焼成することにより欠陥のない高密
度ＩＴＯ焼結体が得られることを見い出した。本発明は
これらの知見に基づいて完成に至ったものである。な
お、ここで言う比表面積は、ＢＥＴ法で測定される値で
ある。Means for Solving the Problems In order to produce a high-density ITO sintered body using recycled ITO powder, the present inventors heat-treated the recycled ITO powder to increase the specific surface area to 2.5 to 7%. It is molded by a slurry casting method using a powder adjusted to a range of 0.02 m 2 / g, dried, and fired in an oxygen atmosphere to obtain a defect-free high-density ITO sintered body. I found something. The present invention has been completed based on these findings. Here, the specific surface area is a value measured by the BET method.
【０００６】本発明は、下記の事項をその特徴としてい
る。 （１）スパッタリング成膜に使用した後のＩＴＯターゲ
ット、あるいは酸化インジウム、酸化錫粉を原料とする
ＩＴＯ焼結体を自生粉砕後、乾燥して得られるＩＴＯリ
サイクル粉を熱処理して比表面積を２．５〜７．０ｍ2
／ｇの範囲に調整し、その粉末を泥漿鋳込み法によって
成形し、得られた成形体を酸素雰囲気で焼成することを
特徴とするＩＴＯリサイクル粉を利用した高密度ＩＴＯ
焼結体の製造方法。The present invention has the following features. (1) An ITO target used after sputtering film formation or an ITO sintered body using indium oxide or tin oxide powder as a raw material is pulverized autogenously and then dried to obtain a recycled ITO powder, which is heat-treated to have a specific surface area of 2%. 0.5-7.0 m 2
/ G, the powder is molded by a slurry casting method, and the obtained molded body is fired in an oxygen atmosphere.
A method for manufacturing a sintered body.
【０００７】[0007]
【発明の実施の形態】以下に、本発明の高密度ＩＴＯ焼
結体の製造方法について詳細に説明する。本発明の、Ｉ
ＴＯリサイクル粉を利用した泥漿鋳込み成形法による高
密度ＩＴＯ焼結体の製造工程は、図１に示す通りであ
る。DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, a method for producing a high-density ITO sintered body of the present invention will be described in detail. In the present invention, I
The manufacturing process of the high-density ITO sintered body by the slip casting method using the recycled TO powder is as shown in FIG.
【０００８】以下に、ＩＴＯ焼結体の製造方法の各製造
工程について説明する。 （ａ）ＩＴＯリサイクル粉の製造 本発明で用いるＩＴＯリサイクル粉は、樹脂ライニング
を施したボールなしのボールミル中にＩＴＯ焼結体の塊
とイオン交換水を入れ自生粉砕を施し、乾燥して得られ
た粉末を原料とする（特開平７−３１６７９８号公
報）。自生粉砕とは、原料自体の大きい塊を粉砕媒体と
して用いる粉砕方法である。[0008] Each of the manufacturing steps of the method for manufacturing an ITO sintered body will be described below. (A) Production of ITO Recycled Powder The ITO recycled powder used in the present invention is obtained by placing a lump of ITO sintered body and ion-exchanged water in a ball mill without a resin-lined ball, performing autogenous pulverization, and drying. The powder thus obtained is used as a raw material (JP-A-7-316798). Autogenous pulverization is a pulverization method using a large lump of the raw material itself as a pulverization medium.
【０００９】（ｂ）熱処理 このＩＴＯリサイクル粉を大気中で熱処理する。熱処理
温度は６００〜９５０℃が好ましい。この熱処理によっ
てＩＴＯリサイクル粉中の微細粒子を粒成長させ、比表
面積を２．５〜７．０ｍ2 ／ｇの範囲に調整すること
で、泥漿鋳込み成形により緻密で均一な成形体を得るこ
とができる。比表面積が２．５ｍ2 ／ｇを下回ると成形
体にクラックや割れが入りやすくなり、一方比表面積が
７．０ｍ2／ｇを上回ると泥漿鋳込み成形時に内部欠陥
が発生しやすくなる。(B) Heat treatment This recycled ITO powder is heat-treated in the air. The heat treatment temperature is preferably from 600 to 950C. By this heat treatment, fine particles in the recycled ITO powder are grown and the specific surface area is adjusted to a range of 2.5 to 7.0 m 2 / g, whereby a dense and uniform molded body can be obtained by slip casting. it can. If the specific surface area is less than 2.5 m 2 / g, cracks and cracks tend to occur in the molded body, while if the specific surface area is more than 7.0 m 2 / g, internal defects tend to occur during the slip casting.
【００１０】熱処理をしない場合、ＩＴＯリサイクル粉
中には微細粒子が多数存在している。微細粒子が多数存
在すると比表面積が増大し、特に比表面積が７．０ｍ2
／ｇを上回るときは、スラリーの鋳込み時においてスラ
リー中の微細粒子が鋳込み型の排水通路となる多孔質部
において目詰まりを起こしやすくなり、その結果、成形
体中の水分の排出が非常に遅くなるか、あるいは全く排
出できなくなり成形体に内部欠陥が発生しやすくなる恐
れがある。反対に過度の熱処理をした場合、粒成長によ
り比表面積が減少し、特に比表面積が２．５ｍ2 ／ｇを
下回るときは、成形体の自然乾燥による収縮が少なくか
つ成形体強度も小さくなるため、乾燥から焼成工程の間
でクラックや割れが発生しやすくなる恐れがある。When heat treatment is not performed, many fine particles are present in the ITO recycled powder. When a large number of fine particles are present, the specific surface area increases, and particularly, the specific surface area is 7.0 m 2.
When the ratio exceeds / g, fine particles in the slurry are liable to cause clogging in the porous portion serving as a drainage passage of the casting mold during the casting of the slurry, and as a result, the discharge of water from the molded body is extremely slow. Or it may not be able to be discharged at all, and internal defects may easily occur in the molded article. On the other hand, when excessive heat treatment is performed, the specific surface area decreases due to grain growth, and particularly when the specific surface area is less than 2.5 m 2 / g, shrinkage due to natural drying of the formed body is small and the strength of the formed body is reduced. In addition, cracks and cracks may be easily generated between the drying and firing steps.
【００１１】（ｃ）スラリー化 樹脂製ポットに粉砕用ボールと熱処理したＩＴＯリサイ
クル粉を入れ、乾式ボールミル混合を行うのが好まし
い。このとき少量のイオン交換水を添加すると、原料粉
のポット壁への付着を減少させ、粉砕混合を十分に行え
る効果が期待できる。次にイオン交換水、分散剤、バイ
ンダーを加え、乾式ボールミルでスラリー化する。(C) Slurry It is preferable to put the milling balls and the heat-recycled ITO recycle powder into a resin pot and mix them with a dry ball mill. At this time, if a small amount of ion-exchanged water is added, the effect of reducing the adhesion of the raw material powder to the pot wall and performing sufficient pulverization and mixing can be expected. Next, ion-exchanged water, a dispersant, and a binder are added, and the mixture is slurried in a dry ball mill.
【００１２】（ｄ）鋳込み成形 スラリーに消泡剤を加えて減圧脱気し、多孔質性の成形
型にスラリーを鋳込み、スラリー中の水分を除くことで
成形体を得る。成形型は、樹脂、石膏、樹脂膜などの多
孔質材料を成形面とし、スラリー中の水分を排出する機
構を有するものなら特に限定されない。(D) Casting molding The slurry is added with an antifoaming agent and degassed under reduced pressure. The slurry is cast into a porous mold, and the molded product is obtained by removing moisture in the slurry. The molding die is not particularly limited as long as it has a molding surface made of a porous material such as resin, gypsum, or a resin film and has a mechanism for discharging water in the slurry.
【００１３】（ｅ）焼成 成形体は焼成に先立ち自然乾燥を行った後、４００〜６
００℃で脱脂を行うのが好ましい。その後、酸素雰囲気
中にて焼成することにより高密度ＩＴＯ焼結体を得る。
焼成温度は１４００〜１６００℃が好ましい。(E) Firing The molded body is naturally dried prior to firing, and then dried for 400 to 6 hours.
It is preferable to perform degreasing at 00 ° C. Thereafter, by firing in an oxygen atmosphere, a high-density ITO sintered body is obtained.
The firing temperature is preferably from 1400 to 1600 ° C.
【００１４】[0014]
【実施例】以下に、本発明を実施例と比較例に基づいて
さらに説明する。実施例１ 自生粉砕により得られた比表面積が１０．２ｍ2 ／ｇで
あるＩＴＯリサイクル粉を、大気中にて７５０℃で３時
間熱処理した。熱処理したＩＴＯリサイクル粉の比表面
積は４．８ｍ2 ／ｇであった。この熱処理したＩＴＯリ
サイクル粉５００ｇ、イオン交換水２５０ｇと直径５ｍ
ｍのジルコニアボールを樹脂製ポットに入れ、２０時間
ボールミル混合を行った。The present invention will be further described below based on examples and comparative examples. Example 1 A recycled ITO powder having a specific surface area of 10.2 m 2 / g obtained by autogenous grinding was heat-treated at 750 ° C. for 3 hours in the atmosphere. The specific surface area of the heat-recycled ITO powder was 4.8 m 2 / g. 500 g of this heat-treated recycled ITO powder, 250 g of ion-exchanged water and a diameter of 5 m
m of zirconia balls were placed in a resin pot and mixed in a ball mill for 20 hours.
【００１５】次に、ポットにイオン交換水９０ｇとポリ
カルボン酸系分散剤５ｇを入れ１時間ボールミル混合し
た。１時間後にワックス系バインダーを５ｇ添加し、１
９時間ボールミル混合を行った。このスラリーを減圧脱
気した。スラリー濃度は８２％であった。尚、スラリー
濃度の定義は次の通りである。 スラリー濃度（％）＝溶質重量／（溶質重量＋溶媒重
量）×１００Next, 90 g of ion-exchanged water and 5 g of a polycarboxylic acid-based dispersant were placed in a pot and mixed in a ball mill for 1 hour. One hour later, 5 g of a wax-based binder was added, and 1
Ball mill mixing was performed for 9 hours. This slurry was degassed under reduced pressure. The slurry concentration was 82%. The definition of the slurry concentration is as follows. Slurry concentration (%) = solute weight / (solute weight + solvent weight) × 100
【００１６】このスラリーを大気圧下で、図２に示すよ
うな内寸法１３０ｍｍφの多孔性樹脂膜型に鋳込み成形
体を得た。成形体を自然乾燥後、６００℃で脱脂処理し
た。脱脂後の密度は、６５．６％（４．６９ｇ／ｃ
ｍ3 ）であった。その後、酸素雰囲気にて１５５０℃で
焼成し、高密度ＩＴＯ焼結体を得た。このときのＩＴＯ
焼結体の寸法は１１２．２ｍｍφ×５．５ｍｍであり、
密度は９８．５％（７．０４ｇ／ｃｍ3 ）であった。This slurry was cast at atmospheric pressure into a porous resin film mold having an inner dimension of 130 mmφ as shown in FIG. After the molded body was naturally dried, it was degreased at 600 ° C. The density after degreasing is 65.6% (4.69 g / c
m 3 ). Then, it was fired at 1550 ° C. in an oxygen atmosphere to obtain a high-density ITO sintered body. ITO at this time
The dimensions of the sintered body are 112.2 mmφ × 5.5 mm,
The density was 98.5% (7.04 g / cm 3 ).
【００１７】実施例２ 自生粉砕により得られた比表面積が１０．０ｍ2 ／ｇで
あるＩＴＯリサイクル粉を大気中にて９００℃で３時間
熱処理した。熱処理したＩＴＯリサイクル粉の比表面積
は３．５ｍ2 ／ｇであった。この熱処理したＩＴＯリサ
イクル粉２５００ｇ、イオン交換水７５ｇと直径５ｍｍ
のジルコニアボールを樹脂製ポットに入れ、２０時間ボ
ールミル混合を行った。 Example 2 A recycled ITO powder having a specific surface area of 10.0 m 2 / g obtained by autogenous pulverization was heat-treated at 900 ° C. for 3 hours in the air. The specific surface area of the heat-treated ITO recycled powder was 3.5 m 2 / g. 2500 g of this heat-treated recycled ITO powder, 75 g of ion-exchanged water and a diameter of 5 mm
Was placed in a resin pot and mixed with a ball mill for 20 hours.
【００１８】次にポットにイオン交換水３８３ｇとポリ
カルボン酸系分散剤１５ｇを入れ、１時間ボールミル混
合した。１時間後にワックス系バインダーを２５ｇ添加
し１９時間ボールミル混合を行った。スラリーにアミド
系消泡剤１．３ｇを添加し減圧脱気を行った。このスラ
リーの濃度は８５％であった。Next, 383 g of ion-exchanged water and 15 g of a polycarboxylic acid-based dispersant were placed in a pot, and mixed in a ball mill for 1 hour. One hour later, 25 g of a wax-based binder was added, and ball mill mixing was performed for 19 hours. 1.3 g of an amide-based antifoaming agent was added to the slurry, and deaeration was performed under reduced pressure. The concentration of this slurry was 85%.
【００１９】このスラリーを圧力１ｋｇ／ｃｍ2 で内寸
法２４５ｍｍ×２４５ｍｍ×９ｍｍの石膏型に鋳込み成
形体を得た。成形体を自然乾燥後、６００℃で脱脂処理
した。脱脂後の密度は、６６．５％（４．７５ｇ／ｃｍ
3 ）であった。その後、酸素雰囲気にて１５５０℃で焼
成し、高密度ＩＴＯ焼結体を得た。このときのＩＴＯ焼
結体の寸法は２１２ｍｍ×２１２ｍｍ×７．５ｍｍであ
り、密度は９９．８％（７．１０ｇ／ｃｍ3 ）であっ
た。This slurry was cast at a pressure of 1 kg / cm 2 into a gypsum mold having an inner size of 245 mm × 245 mm × 9 mm to obtain a molded product. After the molded body was naturally dried, it was degreased at 600 ° C. The density after degreasing is 66.5% (4.75 g / cm
3 ). Then, it was fired at 1550 ° C. in an oxygen atmosphere to obtain a high-density ITO sintered body. At this time, the dimensions of the ITO sintered body were 212 mm × 212 mm × 7.5 mm, and the density was 99.8% (7.10 g / cm 3 ).
【００２０】実施例３ 自生粉砕により得られた比表面積が１０．０ｍ2 ／ｇで
あるＩＴＯリサイクル粉を大気中にて９５０℃で３時間
熱処理した。熱処理したＩＴＯリサイクル粉の比表面積
は２．６ｍ2 ／ｇであった。この熱処理したＩＴＯリサ
イクル粉１０００ｇ、イオン交換水３０ｇと直径５ｍｍ
のジルコニアボールを樹脂製ポットに入れ、２０時間ボ
ールミル混合を行った。 Example 3 A recycled ITO powder having a specific surface area of 10.0 m 2 / g obtained by autogenous grinding was heat-treated at 950 ° C. for 3 hours in the air. The specific surface area of the heat-treated ITO recycled powder was 2.6 m 2 / g. 1000 g of this heat-treated recycled ITO powder, 30 g of ion-exchanged water and a diameter of 5 mm
Was placed in a resin pot and mixed with a ball mill for 20 hours.
【００２１】次に、ポットにイオン交換水１１０ｇとポ
リカルボン酸系分散剤４ｇを入れ、１時間ボールミル混
合した。１時間後にワックス系バインダーを１０ｇ添加
し１９時間ボールミル混合を行った。スラリーにアミド
系消泡剤０．５ｇを添加し減圧脱気を行った。スラリー
濃度は８８％であった。Next, 110 g of ion-exchanged water and 4 g of a polycarboxylic acid-based dispersant were placed in a pot and mixed in a ball mill for 1 hour. One hour later, 10 g of a wax-based binder was added, and ball mill mixing was performed for 19 hours. 0.5 g of an amide-based antifoaming agent was added to the slurry, and deaeration was performed under reduced pressure. The slurry concentration was 88%.
【００２２】このスラリーを大気圧下で、図２に示すよ
うな内寸法１９０ｍｍφの多孔性樹脂膜型に鋳込み成形
体を得た。成形体を自然乾燥後、６００℃で脱脂処理し
た。脱脂後の密度は、６８．１％（４．８７ｇ／ｃ
ｍ3 ）であった。その後、酸素雰囲気にて１５５０℃で
焼成し、高密度ＩＴＯ焼結体を得た。このときのＩＴＯ
焼結体の寸法は１６７ｍｍφ×５．１ｍｍであり、密度
は９７．８％（６．９９ｇ／ｃｍ3 ）であった。This slurry was cast at atmospheric pressure into a porous resin film mold having an inner dimension of 190 mmφ as shown in FIG. After the molded body was naturally dried, it was degreased at 600 ° C. The density after degreasing is 68.1% (4.87 g / c
m 3 ). Then, it was fired at 1550 ° C. in an oxygen atmosphere to obtain a high-density ITO sintered body. ITO at this time
The dimensions of the sintered body were 167 mmφ × 5.1 mm, and the density was 97.8% (6.99 g / cm 3 ).
【００２３】比較例１ 自生粉砕により得られたＩＴＯ粉を熱処理せずに使用し
た。このＩＴＯリサイクル粉の比表面積は１０．０ｍ2
／ｇであった。このＩＴＯリサイクル粉１０００ｇ、イ
オン交換水５５ｇと直径５ｍｍのジルコニアボールを樹
脂製ポットに入れ、２０時間ボールミル混合を行った。
次に、ポットにイオン交換水１９８ｇとポリカルボン酸
系分散剤１１ｇを入れ１時間ボールミル混合した。１時
間後にワックス系バインダーを１１ｇ添加し、１９時間
ボールミル混合を行った。このスラリーに減圧脱気し
た。スラリー濃度は８１％であった。 Comparative Example 1 ITO powder obtained by autogenous grinding was used without heat treatment. The specific surface area of the recycled ITO powder is 10.0 m 2
/ G. 1000 g of the recycled ITO powder, 55 g of ion-exchanged water and zirconia balls having a diameter of 5 mm were placed in a resin pot and mixed with a ball mill for 20 hours.
Next, 198 g of ion-exchanged water and 11 g of a polycarboxylic acid-based dispersant were placed in a pot and mixed in a ball mill for 1 hour. One hour later, 11 g of a wax-based binder was added, and ball mill mixing was performed for 19 hours. This slurry was degassed under reduced pressure. The slurry concentration was 81%.
【００２４】このスラリーを大気圧下で、図２に示すよ
うな内寸法１９０ｍｍφの多孔性樹脂膜型に鋳込み成形
体を得た。成形体を自然乾燥後、６００℃で脱脂処理し
た。脱脂後の密度は、６２．９％（４．５０ｇ／ｃ
ｍ3 ）であった。その後、酸素雰囲気にて１５５０℃で
焼成し、ＩＴＯ焼結体を得た。このときのＩＴＯ焼結体
の寸法は１６１ｍｍφ×６．７ｍｍであり、密度は９
４．３％（６．７４ｇ／ｃｍ3 ）であった。ただし、Ｉ
ＴＯ焼結体に長さ８ｍｍと１１ｍｍの２本のクラックが
発生した。This slurry was cast at atmospheric pressure into a porous resin film mold having an inner dimension of 190 mmφ as shown in FIG. After the molded body was naturally dried, it was degreased at 600 ° C. The density after degreasing is 62.9% (4.50 g / c
m 3 ). Then, it was baked at 1550 ° C. in an oxygen atmosphere to obtain an ITO sintered body. At this time, the size of the ITO sintered body was 161 mmφ × 6.7 mm, and the density was 9 mm.
4.3% (6.74 g / cm 3 ). Where I
Two cracks having a length of 8 mm and 11 mm occurred in the TO sintered body.
【００２５】比較例２ 自生粉砕により得られた比表面積が１０．０ｍ2 ／ｇで
あるＩＴＯリサイクル粉を大気中にて５００℃で３時間
熱処理した。熱処理したＩＴＯリサイクル粉の比表面積
は８．１ｍ2 ／ｇであった。この熱処理したＩＴＯリサ
イクル粉５００ｇ、イオン交換水２５ｇと直径５ｍｍの
ジルコニアボールを樹脂製ポットに入れ、２０時間ボー
ルミル混合を行った。次に、ポットにイオン交換水９０
ｇとポリカルボン酸系分散剤５ｇを入れ１時間ボールミ
ル混合した。１時間後にワックス系バインダーを５ｇ添
加し、１９時間ボールミル混合を行った。このスラリー
を減圧脱気した。スラリー濃度は８２％であった。COMPARATIVE EXAMPLE 2 Recycled ITO powder having a specific surface area of 10.0 m 2 / g obtained by autogenous pulverization was heat-treated in the air at 500 ° C. for 3 hours. The specific surface area of the heat-treated ITO recycled powder was 8.1 m 2 / g. 500 g of the heat-recycled ITO powder, 25 g of ion-exchanged water, and zirconia balls having a diameter of 5 mm were placed in a resin pot, and mixed in a ball mill for 20 hours. Next, 90 ion-exchanged water is added to the pot.
g and 5 g of a polycarboxylic acid-based dispersant were added and mixed in a ball mill for 1 hour. One hour later, 5 g of a wax-based binder was added, and ball mill mixing was performed for 19 hours. This slurry was degassed under reduced pressure. The slurry concentration was 82%.
【００２６】このスラリーを大気圧下で、図２に示すよ
うな内寸法１３０ｍｍφの多孔性樹脂膜型に鋳込み成形
体を得た。成形体を自然乾燥後、６００℃で脱脂処理し
た。脱脂後の密度は、６２．６％（４．４８ｇ／ｃ
ｍ3 ）であった。その後、酸素雰囲気にて１５５０℃で
焼成し、高密度ＩＴＯ焼結体を得た。このときのＩＴＯ
焼結体の寸法は１０９ｍｍφ×６．９ｍｍであり、密度
は９８．２％（７．０２ｇ／ｃｍ3 ）であった。ただ
し、ＩＴＯ焼結体に長さ５ｍｍ〜３０ｍｍの６本のクラ
ックが発生した。This slurry was cast at atmospheric pressure into a porous resin film mold having an inner dimension of 130 mmφ as shown in FIG. After the molded body was naturally dried, it was degreased at 600 ° C. The density after degreasing is 62.6% (4.48 g / c
m 3 ). Then, it was fired at 1550 ° C. in an oxygen atmosphere to obtain a high-density ITO sintered body. ITO at this time
The dimensions of the sintered body were 109 mmφ × 6.9 mm, and the density was 98.2% (7.02 g / cm 3 ). However, six cracks having a length of 5 mm to 30 mm occurred in the ITO sintered body.
【００２７】比較例３ 自生粉砕により得られた比表面積が１０．０ｍ2 ／ｇで
あるＩＴＯリサイクル粉を大気中にて１０００℃で３時
間熱処理した。熱処理したＩＴＯリサイクル粉の比表面
積は２．３ｍ2 ／ｇであった。 Comparative Example 3 An ITO recycled powder having a specific surface area of 10.0 m 2 / g obtained by autogenous pulverization was heat-treated at 1000 ° C. in the air for 3 hours. The specific surface area of the heat-treated ITO recycled powder was 2.3 m 2 / g.
【００２８】この熱処理したＩＴＯリサイクル粉５００
ｇ、イオン交換水２５ｇと直径５ｍｍのジルコニアボー
ルを樹脂製ポットに入れ、２０時間ボールミル混合を行
った。次に、ポットにイオン交換水９０ｇとポリカルボ
ン酸系分散剤５ｇを入れ、１時間ボールミル混合した。
１時間後にワックス系バインダーを５ｇ添加し、１９時
間ボールミル混合を行った。このスラリーを減圧脱気し
た。スラリー濃度は８２％であった。This heat-treated ITO recycled powder 500
g, 25 g of ion-exchanged water and zirconia balls having a diameter of 5 mm were placed in a resin pot and mixed with a ball mill for 20 hours. Next, 90 g of ion-exchanged water and 5 g of a polycarboxylic acid-based dispersant were placed in the pot, and mixed in a ball mill for 1 hour.
One hour later, 5 g of a wax-based binder was added, and ball mill mixing was performed for 19 hours. This slurry was degassed under reduced pressure. The slurry concentration was 82%.
【００２９】このスラリーを大気圧力下で、図２に示す
ような内寸法１３０ｍｍφの多孔性樹脂膜型に鋳込み成
形体を得た。成形体を自然乾燥後、６００℃で脱脂処理
した。脱脂後の密度は、６７．３％（４．８１ｇ／ｃｍ
3 ）であった。その後、酸素雰囲気にて１５５０℃で焼
成し、高密度ＩＴＯ焼結体を得た。このときのＩＴＯ焼
結体の寸法は１０９ｍｍφ×６．９ｍｍであり、密度は
９８．８％（７．０６ｇ／ｃｍ3 ）であった。ただし、
ＩＴＯ焼結体の表面に多数のクラックが発生した。This slurry was cast at atmospheric pressure into a porous resin film mold having an inner dimension of 130 mmφ as shown in FIG. After the molded body was naturally dried, it was degreased at 600 ° C. The density after degreasing is 67.3% (4.81 g / cm
3 ). Then, it was fired at 1550 ° C. in an oxygen atmosphere to obtain a high-density ITO sintered body. At this time, the size of the ITO sintered body was 109 mmφ × 6.9 mm, and the density was 98.8% (7.06 g / cm 3 ). However,
Many cracks occurred on the surface of the ITO sintered body.
【００３０】以上述べた実施例および比較例のデータの
まとめを、表１に示す。自生粉砕により得られたＩＴＯ
リサイクル粉の比表面積が本発明の請求範囲内にある焼
結体は密度が高く、クラック発生も無いことが判る。Table 1 shows a summary of the data of the above-described Examples and Comparative Examples. ITO obtained by autogenous grinding
It can be seen that the sintered body having a specific surface area of the recycled powder within the scope of the present invention has a high density and has no crack.
【００３１】[0031]
【表１】 [Table 1]
【００３２】[0032]
【発明の効果】本発明によれば、ＩＴＯリサイクル粉を
熱処理し、比表面積を２．５〜７．０ｍ2 ／ｇに調製
し、泥漿鋳込み法により成形し、酸素雰囲気で焼成する
ことにより、欠陥がない高密度ＩＴＯ焼結体が得られ
る。According to the present invention, the recycled ITO powder is heat-treated, the specific surface area is adjusted to 2.5 to 7.0 m 2 / g, molded by a slurry casting method, and fired in an oxygen atmosphere. A high-density ITO sintered body without defects can be obtained.
【図１】本発明に係る泥漿鋳込み法による製造工程を示
す説明図である。FIG. 1 is an explanatory view showing a production process by a slurry casting method according to the present invention.
【図２】本発明の泥漿鋳込み法に使用される成形型の説
明図である。FIG. 2 is an explanatory view of a molding die used in the slurry casting method of the present invention.
【符号の説明】 １ スラリー ２ 成形用型枠 ３ 成形用下型 ４ フィルター ５ シール材 ６ 水抜き孔[Explanation of Signs] 1 Slurry 2 Mold frame 3 Mold lower mold 4 Filter 5 Seal material 6 Drain hole
Claims (1)
Ｏ焼結体の製造方法であって、スパッタリング成膜に使
用した後のＩＴＯターゲット、あるいは酸化インジウ
ム、酸化錫を原料とするＩＴＯ焼結体を自生粉砕するこ
とによって粉末とし、次いでこの粉末を熱処理して比表
面積を２．５〜７．０ｍ2 ／ｇの範囲に調整し、その粉
末を泥漿鋳込み成形法によって成形し、得られた成形体
を酸素雰囲気で焼成することを特徴とする、高密度ＩＴ
Ｏ焼結体の製造方法。1. High-density IT using recycled ITO powder
A method for producing an O-sintered body, in which an ITO target used for sputtering film formation or an ITO-sintered body made of indium oxide or tin oxide is spontaneously pulverized into a powder, and then the powder is heat-treated. The specific surface area is adjusted to a range of 2.5 to 7.0 m 2 / g, the powder is molded by a slurry casting method, and the obtained molded body is fired in an oxygen atmosphere. Density IT
A method for producing an O sintered body.
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|---|---|---|---|
| JP02705598A JP4095149B2 (en) | 1998-02-09 | 1998-02-09 | Method for producing high-density ITO sintered body using ITO recycled powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP02705598A JP4095149B2 (en) | 1998-02-09 | 1998-02-09 | Method for producing high-density ITO sintered body using ITO recycled powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH11228219A true JPH11228219A (en) | 1999-08-24 |
| JP4095149B2 JP4095149B2 (en) | 2008-06-04 |
Family
ID=12210396
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP02705598A Expired - Fee Related JP4095149B2 (en) | 1998-02-09 | 1998-02-09 | Method for producing high-density ITO sintered body using ITO recycled powder |
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Cited By (6)
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| WO2010113895A1 (en) * | 2009-03-30 | 2010-10-07 | 住友化学株式会社 | Method for producing aluminum titanate ceramic body |
| WO2010113893A1 (en) * | 2009-03-30 | 2010-10-07 | 住友化学株式会社 | Method for producing aluminum titanate ceramic body |
| WO2011052160A1 (en) * | 2009-10-28 | 2011-05-05 | 株式会社アルバック | Method for producing ito sintered body and method for producing ito sputtering target |
| JP2011519817A (en) * | 2008-05-12 | 2011-07-14 | ビズエスプ リミテッド | Method for producing high-density ITO sputtering target |
| JP2013533391A (en) * | 2010-08-06 | 2013-08-22 | シニト（シェンジェン） オプトエレクトリカル アドヴァンスト マテリアルズ カンパニー リミテッド | Method for producing high-density indium tin oxide (ITO) sputtering target |
| CN113149611A (en) * | 2021-05-17 | 2021-07-23 | 先导薄膜材料（广东）有限公司 | ITO powder prepared by recycling ITO waste target blank, target material and preparation method thereof |
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| JP2011519817A (en) * | 2008-05-12 | 2011-07-14 | ビズエスプ リミテッド | Method for producing high-density ITO sputtering target |
| WO2010113895A1 (en) * | 2009-03-30 | 2010-10-07 | 住友化学株式会社 | Method for producing aluminum titanate ceramic body |
| WO2010113893A1 (en) * | 2009-03-30 | 2010-10-07 | 住友化学株式会社 | Method for producing aluminum titanate ceramic body |
| US8673044B2 (en) | 2009-03-30 | 2014-03-18 | Sumitomo Chemical Company, Limited | Process for producing aluminum titanate-based ceramics body |
| WO2011052160A1 (en) * | 2009-10-28 | 2011-05-05 | 株式会社アルバック | Method for producing ito sintered body and method for producing ito sputtering target |
| JP2011093729A (en) * | 2009-10-28 | 2011-05-12 | Ulvac Japan Ltd | Method for producing ito sintered compact, and method for producing ito sputtering target |
| CN102264666A (en) * | 2009-10-28 | 2011-11-30 | 株式会社爱发科 | Method for producing ito sintered body and method for producing ito sputtering target |
| JP2013533391A (en) * | 2010-08-06 | 2013-08-22 | シニト（シェンジェン） オプトエレクトリカル アドヴァンスト マテリアルズ カンパニー リミテッド | Method for producing high-density indium tin oxide (ITO) sputtering target |
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