JP4075361B2 - Method for producing Mg-containing ITO sputtering target - Google Patents

Method for producing Mg-containing ITO sputtering target Download PDF

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Publication number
JP4075361B2
JP4075361B2 JP2001360793A JP2001360793A JP4075361B2 JP 4075361 B2 JP4075361 B2 JP 4075361B2 JP 2001360793 A JP2001360793 A JP 2001360793A JP 2001360793 A JP2001360793 A JP 2001360793A JP 4075361 B2 JP4075361 B2 JP 4075361B2
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Prior art keywords
powder
mg
magnesium
sputtering target
oxide powder
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Expired - Fee Related
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JP2003160861A (en
Inventor
秀樹 寺岡
裕一 長崎
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東ソー株式会社
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Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for producing a sputtering target used in producing a transparent conductive film.
[0002]
[Prior art]
ITO (Indium Tin Oxide) thin film has characteristics such as high conductivity and high transmittance, and can be easily finely processed. Therefore, display electrodes for flat panel displays, resistive touch panels, solar cell window materials, It is used in a wide range of fields such as antistatic films, electromagnetic wave preventing films, antifogging films, and sensors.
[0003]
Attempts have been made to add a third element for the purpose of giving such an ITO thin film a new function. For example, a method of adding Ta or Hf for the purpose of reducing the resistivity of a thin film, a method of adding Ce for the purpose of reducing the amount of nodule generation, a method of adding C, F, B or the like for the purpose of improving etching characteristics, A method of adding Al and / or Si for the purpose of increasing the resistivity of the thin film can be exemplified.
[0004]
On the other hand, methods for obtaining ITO thin films can be broadly divided into chemical film formation methods such as spray decomposition and CVD, and physical film formation methods such as electron beam evaporation and sputtering. The method is widely used because it is easy to increase the area of the thin film and a high-performance film can be obtained.
[0005]
When ITO film formation by sputtering is performed, if a large amount of arcing occurs, a foreign matter defect occurs in the formed thin film. This causes a decrease in manufacturing yield in flat panel displays such as liquid crystal display devices, and a sputtering target that can suppress arcing is strongly desired.
[0006]
[Problems to be solved by the invention]
The present inventors have developed a method of adding Mg as the third element for the purpose of improving the durability (moisture resistance, high temperature resistance) of the ITO thin film. This Mg-containing ITO thin film has the characteristics that the film surface is flat and the etching characteristics are improved, and the resistivity of the thin film is slightly higher than that of ITO, and it is also excellent in heat resistance and moisture resistance. It has excellent characteristics as a transparent conductive film for a touch panel.
[0007]
A target containing In, Sn, Mg, and O has been manufactured by a method in which indium oxide powder, tin oxide powder and magnesium oxide powder or magnesium hydroxide powder are mixed, molded, and sintered (Japanese Patent Laid-Open No. Hei 10- No. 290610, JP-A-11-270005). However, in such a method, a lot of arcing is generated at the time of sputtering, which has a big problem in terms of manufacturing yield in flat panel displays.
[0008]
An object of the present invention is to solve the above-mentioned problems of the prior art, and to provide a method for producing an Mg-containing ITO sputtering target that substantially consists of In, Sn, Mg, and O and can suppress the occurrence of arcing.
[0009]
[Means for Solving the Problems]
In order to solve the above problems, the present inventors have studied the raw material powder that becomes the Mg source, and as a result, use the magnesium indium oxide powder or the magnesium stannate powder as the raw material powder that becomes the Mg source. The present invention has been completed by finding out what can be done.
[0010]
That is, the present invention provides a method for producing an Mg-containing ITO sputtering target composed of a sintered body substantially composed of In, Sn, Mg and O, and a Mg source in a raw material powder for producing the sintered body. In particular, the present invention relates to a method for producing a Mg-containing ITO sputtering target, characterized in that magnesium indium oxide powder and / or magnesium stannate powder is used as the powder, and in particular, indium oxide powder and tin oxide powder, and magnesium indium oxide powder and / or A method for producing an Mg-containing ITO sputtering target characterized by mixing and shaping with magnesium stannate powder and then sintering to obtain a sintered body substantially composed of In, Sn, Mg and O, and Indium oxide-tin oxide composite oxide powder and magnesium indium oxide powder And / or magnesium stannate powder is mixed, molded, and sintered to obtain a sintered body substantially composed of In, Sn, Mg, and O. It is about.
[0011]
The present invention is described in further detail below.
[0012]
In the method of the present invention, as the raw material powder of the sintered body constituting the Mg-containing ITO sputtering target, for example, (1) a mixture of indium oxide powder, tin oxide powder and magnesium indium acid powder, (2) indium oxide Powder, mixture of tin oxide powder and magnesium stannate powder, (3) Indium oxide powder, tin oxide powder, magnesium indium oxide powder and magnesium stannate powder, (4) Indium oxide-tin oxide composite oxidation Product powder and magnesium indium oxide powder, (5) indium oxide-tin oxide composite oxide powder and magnesium stannate powder, (6) indium oxide-tin oxide composite oxide powder, indium Mixed with magnesium oxide and magnesium stannate powder Or the like can be used. The indium oxide-tin oxide composite oxide powder of the present invention includes: (1) an indium oxide powder in which tin is dissolved; (2) a compound of tin oxide and indium oxide (In 4 Sn 3 O 12 ) powder; 3) Oxide powder such as indium oxide powder, tin oxide powder, indium oxide powder in which tin is dissolved, and / or powder composed of a compound of tin oxide and indium oxide (In 4 Sn 3 O 12 ) powder For example, a mixed powder of indium oxide powder and tin oxide powder is fired and solid phase reacted and then pulverized, or a coprecipitate from a solution containing indium ions and tin ions is calcined and then pulverized. be able to.
[0013]
Here, when a powder other than magnesium indium oxide powder or magnesium stannate powder is used as the magnesium source in the raw material powder, there is a large amount of Mg segregation in the sintered body. In a sputtering target made of such a sintered body, arcing is likely to occur during sputtering.
[0014]
On the other hand, when magnesium indium oxide powder or magnesium stannate powder is used as the magnesium source in the raw material powder, there is no segregation of Mg in the sintered body regardless of the indium source or tin source in the raw material powder. There is an excellent advantage that arcing during sputtering can be suppressed.
[0015]
When manufacturing a Mg-containing ITO sputtering target, a pulverizer such as a ball mill is used to increase the density of the sintered body, and the indium oxide powder, tin oxide powder and magnesium indium oxide powder or magnesium stannate constituting the raw material powder is used. It is desirable to grind the powder so that the maximum particle size is 1 μm or less and the average particle size is 0.4 μm or less. This is the same when the indium oxide-tin oxide composite oxide powder is used or when both the indium magnesium oxide powder and the magnesium stannate powder are used simultaneously. In the present invention, the particle size means the secondary particle size, and the average particle size means the particle size of the powder corresponding to 50% of the cumulative distribution in the volume of the particle size.
[0016]
Here, the mixing amount of the tin oxide powder in the raw material powder is set to such a mixing amount that Sn / (Sn + In) is 1.9 to 14% by atomic ratio with respect to Sn and In in the obtained sintered body. It is preferable. More preferably, it is 4 to 11%. If it exists in this range, when manufacturing a Mg containing ITO thin film using the target obtained by the method of this invention, the resistivity of the thin film obtained can be reduced most.
[0017]
The mixing amount of the magnesium indium oxide powder or the magnesium stannate powder in the raw material powder is such that Mg / (In + Sn + Mg) is 0.1 to 20.0% by atomic ratio with respect to Sn, In and Mg in the obtained sintered body. It is preferable to set it as the mixing amount. More preferably, it is 0.1-15.0%, More preferably, it is 0.5-13.0%. If Mg / (In + Sn + Mg) in the obtained sintered body is less than 0.1%, the etching characteristics and durability may be inferior and may not be appropriate. If it exceeds 20.0%, the resistivity may be too high. is there. When the evaporation of Sn, In, and Mg in the raw material powder during sintering cannot be ignored, the mixing ratio of the raw material powder is adjusted in consideration of a composition shift due to evaporation. The same applies when mixing both the magnesium indium oxide powder and the magnesium stannate powder as the raw material powder.
[0018]
The raw material powders may be mixed by dry mixing or wet mixing by a known method such as a ball mill.
[0019]
Next, an Mg-containing ITO sputtering target made of an Mg-containing ITO sintered body is produced using the obtained mixed powder. Although it does not specifically limit about the manufacturing method of Mg containing ITO sintered compact, For example, it can manufacture by the following methods.
[0020]
A binder is added to the mixed powder of indium oxide powder, tin oxide powder and magnesium indium oxide powder or magnesium stannate powder obtained as described above, and molding is performed by a molding method such as pressing or casting. Thus, a molded body is manufactured.
[0021]
In the case of producing a molded body by the pressing method, after a predetermined mold is filled with the mixed powder, pressing is performed at a pressure of 100 to 300 kg / cm 2 using a powder pressing machine. When the moldability of the powder is poor, a binder such as paraffin or polyvinyl alcohol may be added as necessary.
[0022]
When manufacturing a molded body by a casting method, a binder, a dispersant, and ion-exchanged water are added to the mixed powder of indium oxide powder, tin oxide powder and magnesium indium oxide powder or magnesium stannate powder, which are the raw material powders described above. Then, a slurry for producing a cast product is produced by mixing with a ball mill or the like. Subsequently, casting is performed using the obtained slurry. It is preferable to defoam the slurry before injecting the slurry into the mold. Defoaming may be performed, for example, by adding a polyalkylene glycol antifoaming agent to the slurry and performing defoaming treatment in a vacuum. Subsequently, the cast molding is dried.
[0023]
Next, the obtained compact is subjected to densification treatment such as cold isostatic pressing (CIP) as necessary. Here CIP pressure is preferably 2 ton / cm 2 or more to obtain a sufficient consolidation effect is more preferably a 2~5ton / cm 2.
[0024]
Here, when the first molding is performed by a casting method, a binder removal treatment may be performed for the purpose of removing moisture remaining in the molded body after CIP and organic substances such as a binder. Even when the first molding is performed by the press method, it is desirable to perform the same debinding process when a binder is used during molding.
[0025]
The molded body thus obtained is put into a sintering furnace and sintered. Any method can be used as the sintering method, but in the air, considering the cost of production equipment, etc., it is desirable to sinter in air. In addition to this, it goes without saying that other conventionally known sintering methods such as a hot press (HP) method, a hot isostatic press (HIP) method and an oxygen pressure sintering method can be used.
[0026]
Sintering conditions can also be selected as appropriate, but when producing an Mg-containing ITO sputtering target, the sintering temperature is 1450 to 1650 ° C. in order to obtain a sufficient density increasing effect and to suppress the evaporation of tin oxide. It is desirable that The atmosphere during sintering is preferably air or a pure oxygen atmosphere. Further, the sintering time is preferably 5 hours or more in order to obtain a sufficient density increasing effect, and more preferably 5 to 30 hours.
[0027]
Next, the obtained sintered body is processed into a desired shape by machining or the like, and the processed Mg-containing ITO sintered body is used as necessary, for example, with an indium solder on a backing plate made of oxygen-free copper. The Mg-containing ITO sputtering target is manufactured by bonding.
[0028]
【Example】
EXAMPLES Hereinafter, although an Example demonstrates this invention further in detail, this invention is not limited to these.
[0029]
Example 1
450 parts by weight of In 2 O 3 powder (average particle size 0.38 μm), 50 parts by weight of SnO 2 powder (average particle size 0.38 μm) and 30 parts by weight of magnesium indium acid powder (average particle size 0.40 μm) are made of polyethylene. And mixed with a dry ball mill for 72 hours to produce a mixed powder.
[0030]
This powder was put into a mold and pressed at a pressure of 300 kg / cm 2 to obtain a molded body. The size of the compacts was 150 mm × 300 mm × 10 mmt, and these compacts were densified with CIP at a pressure of 3 ton / cm 2 . Next, the compact was placed in a pure oxygen atmosphere sintering furnace and sintered under the following conditions.
(Sintering conditions)
Sintering temperature: 1500 ° C., heating rate: 25 ° C./Hr, sintering time: 6 hours, oxygen pressure: 50 mmH 2 O (gauge pressure), oxygen linear velocity (oxygen inflow rate / sintering furnace floor area): 2 The obtained sintered body was processed into a 100 mm × 200 mm × 6 mmt sintered body by a wet processing method, and bonded to an oxygen-free copper backing plate using indium solder to obtain a target. Sputtering was performed using this target under the following conditions.
Equipment: DC magnetron sputtering equipment Magnetic field strength: 1000 Gauss (horizontal component directly above the target)
Sputtering gas: Ar + O 2
Sputtering gas pressure: 5 mTorr
O 2 / Ar: 0.6% (volume ratio)
DC power: 600W
The number of arcing generated during the continuous discharge for 30 hours was 103 times.
[0031]
Example 2
450 parts by weight of In 2 O 3 powder (average particle size 0.38 μm), 50 parts by weight of SnO 2 powder (average particle size 0.38 μm) and 30 parts by weight of magnesium stannate powder (average particle size 0.40 μm) are made of polyethylene And mixed with a dry ball mill for 72 hours to produce a mixed powder.
[0032]
This powder was put into a mold and pressed at a pressure of 300 kg / cm 2 to obtain a molded body. The size of the compacts was 150 mm × 300 mm × 10 mmt, and these compacts were densified with CIP at a pressure of 3 ton / cm 2 .
[0033]
The molded body was sintered under the same conditions as in Example 1.
[0034]
This sintered body was processed into a 100 mm × 200 mm × 6 mmt sintered body by a wet processing method, and bonded to a backing plate made of oxygen-free copper using indium solder to obtain a target. The obtained target was sputtered under the same conditions as in Example 1, and the number of arcing occurrences was examined.
[0035]
The arcing number at the end of the discharge was 105 times.
[0036]
Example 3
500 parts by weight of indium oxide-tin oxide composite oxide powder (average particle size 0.38 μm) and 30 parts by weight of magnesium stannate powder (average particle size 0.40 μm) prepared by coprecipitation method are put in a polyethylene pot. Then, it was mixed for 72 hours by a dry ball mill to produce a mixed powder.
[0037]
This powder was put into a mold and pressed at a pressure of 300 kg / cm 2 to obtain a molded body. The size of the compacts was 150 mm × 300 mm × 10 mmt, and these compacts were densified with CIP at a pressure of 3 ton / cm 2 .
[0038]
The molded body was sintered under the same conditions as in Example 1.
[0039]
This sintered body was processed into a 100 mm × 200 mm × 6 mmt sintered body by a wet processing method, and bonded to a backing plate made of oxygen-free copper using indium solder to obtain a target. The obtained target was sputtered under the same conditions as in Example 1, and the number of arcing occurrences was examined.
[0040]
The arcing number at the end of the discharge was 104 times.
[0041]
Example 4
450 parts by weight of In 2 O 3 powder (average particle size 0.38 μm), 50 parts by weight of SnO 2 powder (average particle size 0.38 μm), 15 parts by weight of magnesium indium acid powder (average particle size 0.40 μm) and stannic acid 15 parts by weight of magnesium powder (average particle size 0.40 μm) was placed in a polyethylene pot and mixed by a dry ball mill for 72 hours to produce a mixed powder.
[0042]
This powder was put into a mold and pressed at a pressure of 300 kg / cm 2 to obtain a molded body. The size of the compacts was 150 mm × 300 mm × 10 mmt, and these compacts were densified with CIP at a pressure of 3 ton / cm 2 .
[0043]
The molded body was sintered under the same conditions as in Example 1.
[0044]
This sintered body was processed into a 100 mm × 200 mm × 6 mmt sintered body by a wet processing method, and bonded to a backing plate made of oxygen-free copper using indium solder to obtain a target. The obtained target was sputtered under the same conditions as in Example 1, and the number of arcing occurrences was examined.
[0045]
The arcing number at the end of the discharge was 102 times.
[0046]
Comparative Example 1
450 parts by weight of In 2 O 3 powder (average particle size 0.38 μm), 50 parts by weight of SnO 2 powder (average particle size 0.38 μm) and 30 parts by weight of magnesium oxide powder (average particle size 0.40 μm) are made of polyethylene. It put into the pot and mixed for 72 hours with the dry-type ball mill, and mixed powder was manufactured.
[0047]
This powder was put into a mold and pressed at a pressure of 300 kg / cm 2 to obtain a molded body. The size of the compacts was 150 mm × 300 mm × 10 mmt, and these compacts were densified with CIP at a pressure of 3 ton / cm 2 .
[0048]
The molded body was sintered under the same conditions as in Example 1.
[0049]
This sintered body was processed into a 100 mm × 200 mm × 6 mmt sintered body by a wet processing method, and bonded to a backing plate made of oxygen-free copper using indium solder to obtain a target. The obtained target was sputtered under the same conditions as in Example 1, and the number of arcing occurrences was examined.
[0050]
The arcing number at the end of the discharge was 986 times.
[0051]
Comparative Example 2
450 parts by weight of In 2 O 3 powder (average particle size 0.38 μm), 50 parts by weight of SnO 2 powder (average particle size 0.38 μm) and 30 parts by weight of magnesium hydroxide powder (average particle size 0.40 μm) are made of polyethylene And mixed with a dry ball mill for 72 hours to produce a mixed powder.
[0052]
This powder was put into a mold and pressed at a pressure of 300 kg / cm 2 to obtain a molded body. The size of the compacts was 150 mm × 300 mm × 10 mmt, and these compacts were densified with CIP at a pressure of 3 ton / cm 2 .
[0053]
The molded body was sintered under the same conditions as in Example 1.
[0054]
This sintered body was processed into a 100 mm × 200 mm × 6 mmt sintered body by a wet processing method, and bonded to a backing plate made of oxygen-free copper using indium solder to obtain a target. The obtained target was sputtered under the same conditions as in Example 1, and the number of arcing occurrences was examined.
[0055]
The arcing number at the end of the discharge was 1002.
[0056]
【The invention's effect】
As described above, according to the present invention, it is possible to produce an Mg-containing ITO sputtering target capable of suppressing the occurrence of arcing by using magnesium indium oxide powder or magnesium stannate powder as the Mg source of the Mg-containing ITO sputtering target. it can.

Claims (4)

  1. In the manufacturing method of Mg containing ITO sputtering target comprised from the sintered compact which consists of In , Sn, Mg, and O, as a powder used as the Mg source in the raw material powder for manufacturing the said sintered compact, magnesium indium acid powder And / or the manufacturing method of Mg containing ITO sputtering target characterized by using magnesium stannate powder.
  2. Indium oxide powder and tin oxide powder and magnesium indium oxide powder and / or magnesium stannate powder are mixed and molded, and then sintered to obtain a sintered body made of In , Sn, Mg and O. A method for producing an Mg-containing ITO sputtering target.
  3. Indium oxide-tin oxide composite oxide powder, magnesium indium oxide powder and / or magnesium stannate powder are mixed and molded, and then sintered to obtain a sintered body made of In , Sn, Mg and O. The manufacturing method of Mg containing ITO sputtering target characterized by these.
  4. The content of Mg in the sintered body is a proportion of 0.1 to 20.0% in terms of an atomic ratio of Mg / (In + Sn + Mg). Manufacturing method of Mg containing ITO sputtering target.
JP2001360793A 2001-11-27 2001-11-27 Method for producing Mg-containing ITO sputtering target Expired - Fee Related JP4075361B2 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011058645A1 (en) * 2009-11-13 2011-05-19 三菱重工業株式会社 Machine tool control method and control device
KR20180014037A (en) 2016-03-14 2018-02-07 제이엑스금속주식회사 Oxide sintered compact

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009001693A1 (en) 2007-06-26 2008-12-31 Nippon Mining & Metals Co., Ltd. Amorphous composite oxide film, crystalline composite oxide film, process for producing amorphous composite oxide film, process for producing crystalline composite oxide film, and composite oxide sinter
KR101155358B1 (en) 2007-07-13 2012-06-19 제이엑스 닛코 닛세키 킨조쿠 가부시키가이샤 Composite oxide sinter, process for producing amorphous composite oxide film, amorphous composite oxide film, process for producing crystalline composite oxide film, and crystalline composite oxide film
KR20100063137A (en) * 2007-10-03 2010-06-10 미츠이 긴조쿠 고교 가부시키가이샤 Indium oxide target
JP5377328B2 (en) * 2007-12-25 2013-12-25 出光興産株式会社 Tin oxide-magnesium oxide sputtering target and transparent semiconductor film

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011058645A1 (en) * 2009-11-13 2011-05-19 三菱重工業株式会社 Machine tool control method and control device
CN102596495A (en) * 2009-11-13 2012-07-18 三菱重工业株式会社 Machine tool control method and control device
KR20180014037A (en) 2016-03-14 2018-02-07 제이엑스금속주식회사 Oxide sintered compact

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