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Definitions

• the present invention relates to a target for forming an optical thin film that does not contain sulfur, has low bulk resistance, can be DC-sputtered, and has a low refractive index, and a method for manufacturing the same.
• ZnS—SiO 2 which is generally used mainly for a protective layer of a phase change type optical information recording medium has excellent characteristics in optical characteristics, thermal characteristics, adhesion to the recording layer, etc. in use.
• rewritable optical disks represented by Blu-Ray are now strongly required to increase the number of rewrites, increase the capacity, and increase the recording speed.
• One of the causes of deterioration of the number of rewrites of the optical information recording medium is diffusion of sulfur components from ZnS—SiO 2 to the recording layer material arranged so as to be sandwiched between the protective layers ZnS—SiO 2. .
• pure Ag or an Ag alloy having high reflectivity and high thermal conductivity has been used for the reflective layer material in order to increase the capacity and increase the recording speed.
• Such a reflective layer is also a protective layer material. It is arranged so as to be in contact with ZnS—SiO 2 .
• the pure Ag or Ag alloy reflective layer material also corrodes and becomes a factor that causes the characteristics such as the reflectance of the optical information recording medium to deteriorate. It was.
• an intermediate layer mainly composed of nitride or carbide is provided between the reflective layer and the protective layer and between the recording layer and the protective layer.
• the protective layer material is replaced with an oxide-only material that does not contain sulfides, and a material system having optical characteristics equal to or better than ZnS-SiO 2 and amorphous stability is studied. Has been.
• a ceramic target such as ZnS—SiO 2 has a high bulk resistance value, it cannot be formed by a direct current sputtering apparatus, and a high frequency sputtering (RF) apparatus is usually used.
• RF high frequency sputtering
• this high-frequency sputtering (RF) apparatus has not only an expensive apparatus itself, but also has a number of disadvantages such as poor sputtering efficiency, large power consumption, complicated control, and slow film formation speed.
• RF high frequency sputtering
• ZnS—SiO 2 has a large film thickness, there has been a problem of a decrease in throughput and an increase in cost.
• a ZnO sputtering target has been proposed under the condition that at least one element to be added is dissolved in ZnO (see Patent Document 3). Since this is a condition that the additive element is dissolved, there is a problem that the component composition is limited, and therefore the optical characteristics are also limited.
• Patent Document 4 that is, Al 2 O 3 : 0.2 to 3.0 at%, MgO and / or SiO 2 : 1 to 27 at%.
• a sputtering target having a low refractive index and a low bulk resistance made of the remaining ZnO, the target and the film formation characteristics could be greatly improved.
• Patent Document 4 is a sputtering target capable of forming a film having a low refractive index.
• the present invention provides a sintered body capable of forming a thin film having a low refractive index by DC sputtering and a method for producing the same. As a result, it is possible to increase the deposition rate, and to significantly improve the throughput of forming a thin film having a low refractive index.
• the present inventors have conducted intensive research. As a result, low bulk resistance is achieved by sintering in an inert gas or vacuum atmosphere even in a low refractive index composition region. And obtained knowledge that DC sputtering is possible. And the high-speed film-forming by DC sputtering was attained, and the knowledge that the characteristic improvement and productivity improvement of an optical information recording medium were possible was acquired.
• the present invention is based on this finding, 1) It consists of zinc (Zn), aluminum (Al), magnesium (Mg) and / or silicon (Si), oxygen (O), and the Al content is 0.1 to 3.0 mol in terms of Al 2 O 3. %, Mg and / or 27 ⁇ 70 mol% total content of MgO and / or SiO 2 in terms of Si, sintered, wherein the balance of the content of ZnO conversion Zn. 2) The sintered body according to 1) above, wherein the sintered body has a bulk resistance of 10 ⁇ ⁇ cm or less. 3) The sintered body according to 1) or 2) above, wherein the relative density is 90% or more. 4) A metal that further forms an oxide having a melting point of 1000 ° C.
• the oxide selected from B 2 O 3, P 2 O 5, K 2 O, V 2 O 5, Sb 2 O 3, TeO 2, Ti 2 O 3, PbO, Bi 2 O 3, MoO 3
• the sintered body according to 4) above which is one or more kinds of materials.
• Al 2 O 3 powder is 0.1 to 3.0 mol%
• MgO and / or SiO 2 powder is 27 to 70 mol%
• the balance is ZnO powder
• these raw material powders are adjusted so that the total amount becomes 100 mol%.
• a method for producing a sintered body comprising adjusting and sintering the raw material powder in an inert gas or vacuum atmosphere at 1050 ° C. or higher and 1500 ° C. or lower. 9) The method for producing a sintered body according to 8) above, further comprising adding 0.1 to 5 wt% of an oxide powder having a melting point of 1000 ° C. or less to obtain a raw material powder.
• the present invention has an excellent effect that it is possible to provide a sintered body capable of forming a thin film having a low refractive index by DC sputtering and a method for manufacturing the same.
• a sputtering target that is particularly useful for a thin film for an optical information recording medium (particularly for use as a protective film, a reflective layer, or a semi-transmissive film layer).
• the present invention is a sintered body having zinc (Zn), aluminum (Al), magnesium (Mg) and / or silicon (Si), and oxygen (O) as constituent elements, and the Al content is Al 2 O. 3 0.1 ⁇ 3.0 mol% in terms of, Mg and / or 27 ⁇ 70 mol% total content of MgO and / or SiO 2 in terms of Si, a content of ZnO in terms of the balance Zn, DC It has a low bulk resistance that allows sputtering. In adjusting the raw materials, the balance is adjusted so that the balance of each oxide is 100 mol% with the balance being ZnO, and therefore the Zn content can be determined from the balance of ZnO.
• each metal in a sintered compact exists in part or all as complex oxide.
• each content is measured not as an oxide but as a metal.
• the sintered body of the present invention is characterized by adding 0.1 to 3.0 mol% of an oxide of Al in terms of Al 2 O 3 in order to impart conductivity. Addition of an Al oxide exceeding this range makes it difficult to impart desired conductivity.
• the sintered body of the present invention is characterized by adding an oxide of Mg and / or Si in order to lower the refractive index. MgO and SiO 2 can be added individually or in combination, respectively, and both can achieve the object of the present invention.
• the sintered body of the present invention has a bulk resistance value that allows DC sputtering, but is more preferably 10 ⁇ ⁇ cm or less. More preferably, it is 1 ⁇ ⁇ cm or less.
• the sintered body of the present invention preferably has a relative density of 90% or more. By setting the relative density to 90% or more, the film thickness uniformity of the thin film formed by sputtering can be improved.
• the present invention is characterized by containing 0.1 to 5 wt% of a metal forming an oxide having a melting point of 1000 ° C. or less in terms of oxide.
• a metal forming an oxide having a melting point of 1000 ° C. or less in terms of oxide.
• this low melting point oxide especially from B 2 O 3 , P 2 O 5 , K 2 O, V 2 O 5 , Sb 2 O 3 , TeO 2 , Ti 2 O 3 , PbO, Bi 2 O 3 , MoO 3
• Addition of selected materials is effective. If the content is less than 0.1 wt%, the above effect cannot be obtained sufficiently, and if it exceeds 5 wt%, the properties are affected depending on the composition, which is not preferable.
• the sintered compact sputtering target of the present invention is useful for industrially producing an optical thin film for an optical disc having a refractive index of 2.00 or less with respect to light having a wavelength of 550 nm.
• it can be used as a target for forming a protective layer, a reflective layer, or a semi-transmissive layer of an optical information recording medium.
• the raw material Al 2 O 3 powder is 0.1 to 3.0 mol%, MgO and / or SiO 2 powder is 27 to 70 mol%, and the balance is ZnO powder. %,
• the basic raw material powder is adjusted, and this mixed powder is sintered at 1050 ° C. or higher and 1500 ° C. or lower.
• Of particular importance in the present invention is sintering under an inert gas or vacuum atmosphere. Sintering in an inert gas or vacuum atmosphere causes oxygen vacancies in part of ZnO. Due to this oxygen deficiency, conductivity can be obtained, and a sintered body having a low bulk resistance capable of DC sputtering can be produced.
• As the atmospheric gas there are argon gas, nitrogen gas and the like, and those generally used as so-called inert atmosphere can be used.
• the Al 2 O 3 powder and the ZnO powder as raw materials are preliminarily mixed and pre-calcined, and then the pre-sintered Al 2 O 3 —ZnO powder (AZO powder) is mixed with MgO and / or SiO 2 powder. Can also be mixed and sintered.
• AZO powder pre-sintered Al 2 O 3 —ZnO powder
• MgO and / or SiO 2 powder Al 2 O 3 and MgO and / or SiO 2 are likely to react to form spinel, and the bulk resistance value tends to increase. Therefore, in order to achieve a lower bulk resistance of the sintered body, it is desired to sinter using a pre-sintered Al 2 O 3 —ZnO content (AZO powder).
• the raw material Al 2 O 3 powder and ZnO powder are mixed in advance and preliminarily calcined to obtain AZO powder, and the raw material MgO powder and SiO 2 powder are similarly mixed and calcined.
• the MgO—SiO 2 calcined powder be mixed with the calcined Al 2 O 3 —ZnO powder (AZO powder) and sintered. This is because spinelization can be further suppressed and low bulk resistance can be achieved.
• 0.1 to 5 wt% of a low melting point oxide powder having a melting point of 1000 ° C. or lower can be added to obtain a raw material for sintering. It is also effective to mix this low melting point oxide powder with the calcined powder previously mixed and calcined.
• the sintered body having such a component composition can retain electrical conductivity, and a thin film can be formed by direct current sputtering (DC sputtering).
• DC sputtering is superior to RF sputtering in that the deposition rate is high and sputtering efficiency is good, and the throughput can be significantly improved.
• the DC sputtering apparatus is advantageous in that it is inexpensive, easy to control, and consumes less power. Since it is possible to reduce the thickness of the protective film itself, it is possible to further improve productivity and prevent substrate heating.
• Example 1 3N equivalent ZnO powder of 5 ⁇ m or less, 3N equivalent of MgO powder with an average particle size of 5 ⁇ m or less, 3N equivalent of Al 2 O 3 powder with an average particle size of 5 ⁇ m or less, 3N equivalent of SiO 2 powder with an average particle size of 5 ⁇ m or less
• Table 1 after adjusting the ratio of the basic raw materials so that the total amount becomes 100 mol% as shown in Table 1, the average particle diameter is 5 ⁇ m corresponding to 3N which is a low melting point oxide having a melting point of 1000 ° C. or less.
• the following B 2 O 3 powder was prepared at the ratio shown in Table 1. Next, after mixing this, it hot-pressed (HP) at the temperature of 1050 degreeC by argon atmosphere. The pressure of the hot press was 220 kg / cm 2 .
• the sintered body was finished into a target shape by machining.
• the density of the sintered compact target reached 100.0%, and the bulk resistance was 3.2 ⁇ 10 ⁇ 3 ⁇ ⁇ cm (3.2 m ⁇ ⁇ cm).
• the density displayed in this specification means a relative density.
• Each relative density is obtained by measuring the density of a target, which is a produced complex oxide, with respect to the theoretical density of the target calculated from the density of the raw material, and obtaining the relative density from each density. Since it is not a simple mixture of raw materials, as shown in Table 1, there is an example in which the relative density exceeds 100%.
• Sputtering was performed using the above-mentioned 6-inch ⁇ -sized target that was finished.
• the sputtering conditions were DC sputtering, sputtering power 500 W, Ar-2% O 2 mixed gas pressure 0.5 Pa, and a film thickness of 1500 mm was formed.
• the film formation rate was 2.8 ⁇ / sec, stable DC sputtering was possible, and good sputtering properties were obtained.
• Example 2 3N equivalent ZnO powder of 5 ⁇ m or less, 3N equivalent of MgO powder with an average particle size of 5 ⁇ m or less, 3N equivalent of Al 2 O 3 powder with an average particle size of 5 ⁇ m or less, 3N equivalent of SiO 2 powder with an average particle size of 5 ⁇ m or less
• Table 1 after adjusting the ratio of the basic raw materials so that the total amount becomes 100 mol% as shown in Table 1, the average particle diameter is 5 ⁇ m corresponding to 3N which is a low melting point oxide having a melting point of 1000 ° C. or less.
• the following B 2 O 3 powder was prepared at the ratio shown in Table 1. Next, after mixing this, it hot-pressed (HP) at the temperature of 1050 degreeC by argon atmosphere. The pressure of the hot press was 220 kg / cm 2 .
• the sintered body was finished into a target shape by machining.
• the density of the sintered compact target reached 99.5%, and the bulk resistance was 2.9 ⁇ 10 ⁇ 3 ⁇ ⁇ cm (2.9 m ⁇ ⁇ cm).
• sputtering was performed under the same conditions as in Example 1 using the above-finished 6-inch ⁇ target. As a result, stable DC sputtering was possible and good sputtering properties were obtained.
• Table 1 after adjusting the ratio of the basic raw materials so that the total amount becomes 100 mol% as shown in Table 1, the average particle diameter is 5 ⁇ m corresponding to 3N which is a low melting point oxide having a melting point of 1000 ° C. or less.
• the following B 2 O 3 powder was prepared at the ratio shown in Table 1. Next, after mixing this, it hot-pressed (HP) at the temperature of 1050 degreeC by argon atmosphere. The pressure of the hot press was 220 kg / cm 2 .
• the sintered body was finished into a target shape by machining.
• the density of the sintered compact target reached 99.8%, and the bulk resistance was 3.0 ⁇ 10 ⁇ 3 ⁇ ⁇ cm (3.0 m ⁇ ⁇ cm).
• sputtering was performed under the same conditions as in Example 1 using the above-finished 6-inch ⁇ target. As a result, stable DC sputtering was possible and good sputtering properties were obtained.
• Example 4 3N equivalent ZnO powder of 5 ⁇ m or less, 3N equivalent of MgO powder with an average particle size of 5 ⁇ m or less, 3N equivalent of Al 2 O 3 powder with an average particle size of 5 ⁇ m or less, 3N equivalent of SiO 2 powder with an average particle size of 5 ⁇ m or less
• Table 1 after adjusting the ratio of the basic raw materials so that the total amount becomes 100 mol% as shown in Table 1, the average particle diameter is 5 ⁇ m corresponding to 3N which is a low melting point oxide having a melting point of 1000 ° C. or less.
• the following B 2 O 3 powder was prepared at the ratio shown in Table 1. Next, after mixing this, it hot-pressed (HP) at the temperature of 1050 degreeC by argon atmosphere. The pressure of the hot press was 220 kg / cm 2 .
• the sintered body was finished into a target shape by machining.
• the density of the sintered compact target reached 107.9%, and the bulk resistance was 3.7 ⁇ 10 ⁇ 1 ⁇ ⁇ cm (0.37 m ⁇ ⁇ cm).
• sputtering was performed under the same conditions as in Example 1 using the above-finished 6-inch ⁇ target. As a result, stable DC sputtering was possible and good sputtering properties were obtained.
• Example 5 3N equivalent ZnO powder of 5 ⁇ m or less, 3N equivalent of MgO powder with an average particle size of 5 ⁇ m or less, 3N equivalent of Al 2 O 3 powder with an average particle size of 5 ⁇ m or less, 3N equivalent of SiO 2 powder with an average particle size of 5 ⁇ m or less
• Table 1 after adjusting the ratio of the basic raw materials so that the total amount becomes 100 mol% as shown in Table 1, the average particle diameter is 5 ⁇ m corresponding to 3N which is a low melting point oxide having a melting point of 1000 ° C. or less.
• the following B 2 O 3 powder was prepared at the ratio shown in Table 1. Next, after mixing this, it hot-pressed (HP) at the temperature of 1050 degreeC by argon atmosphere. The pressure of the hot press was 220 kg / cm 2 .
• the sintered body was finished into a target shape by machining.
• the density of the sintered compact target reached 98.1%, and the bulk resistance was 9.0 ⁇ 10 ⁇ 1 ⁇ ⁇ cm (0.9 ⁇ ⁇ cm).
• sputtering was performed under the same conditions as in Example 1 using the above-finished 6-inch ⁇ target. As a result, stable DC sputtering was possible and good sputtering properties were obtained.
• Example 6 3N equivalent ZnO powder of 5 ⁇ m or less, 3N equivalent of MgO powder with an average particle size of 5 ⁇ m or less, 3N equivalent of Al 2 O 3 powder with an average particle size of 5 ⁇ m or less, 3N equivalent of SiO 2 powder with an average particle size of 5 ⁇ m or less
• Table 1 after adjusting the ratio of the basic raw materials so that the total amount becomes 100 mol% as shown in Table 1, the average particle diameter is 5 ⁇ m corresponding to 3N which is a low melting point oxide having a melting point of 1000 ° C. or less.
• the following B 2 O 3 powder was prepared at the ratio shown in Table 1. Next, after mixing this, it hot-pressed (HP) at the temperature of 1050 degreeC by argon atmosphere. The pressure of the hot press was 220 kg / cm 2 .
• the sintered body was finished into a target shape by machining.
• the density of the sintered compact target reached 101.5%, and the bulk resistance was 2.8 ⁇ 10 ⁇ 3 ⁇ ⁇ cm (2.8 m ⁇ ⁇ cm).
• sputtering was performed under the same conditions as in Example 1 using the above-finished 6-inch ⁇ target. As a result, stable DC sputtering was possible and good sputtering properties were obtained.
• Example 7 3N equivalent ZnO powder of 5 ⁇ m or less, 3N equivalent of MgO powder with an average particle size of 5 ⁇ m or less, 3N equivalent of Al 2 O 3 powder with an average particle size of 5 ⁇ m or less, 3N equivalent of SiO 2 powder with an average particle size of 5 ⁇ m or less
• the raw materials were used, and as shown in Table 1, the ratio of the basic raw materials was adjusted so that the total amount was 100 mol%. Next, after mixing this, it hot-pressed (HP) at the temperature of 1200 degreeC by argon atmosphere. The pressure of the hot press was 220 kg / cm 2 .
• the sintered body was finished into a target shape by machining.
• the density of the sintered compact target reached 97.8%, and the bulk resistance was 1.6 ⁇ 10 ⁇ 3 ⁇ ⁇ cm (1.6 m ⁇ ⁇ cm).
• sputtering was performed under the same conditions as in Example 1 using the above-finished 6-inch ⁇ target. As a result, stable DC sputtering was possible and good sputtering properties were obtained.
• Example 8 3N equivalent ZnO powder of 5 ⁇ m or less, 3N equivalent of MgO powder with an average particle size of 5 ⁇ m or less, 3N equivalent of Al 2 O 3 powder with an average particle size of 5 ⁇ m or less, 3N equivalent of SiO 2 powder with an average particle size of 5 ⁇ m or less
• Table 1 after adjusting the ratio of the basic raw materials so that the total amount becomes 100 mol% as shown in Table 1, the average particle diameter is 5 ⁇ m corresponding to 3N which is a low melting point oxide having a melting point of 1000 ° C. or less.
• the following B 2 O 3 powder was prepared at the ratio shown in Table 1. Next, after mixing this, it sintered at the temperature of 1400 degreeC by nitrogen atmosphere.
• the sintered body was finished into a target shape by machining.
• the density of the sintered compact target reached 94.5%, and the bulk resistance was 3.0 ⁇ 10 ⁇ 3 ⁇ ⁇ cm (3.0 m ⁇ ⁇ cm).
• sputtering was performed under the same conditions as in Example 1 using the above-finished 6-inch ⁇ target. As a result, stable DC sputtering was possible and good sputtering properties were obtained.
• the sintered body was finished into a target shape by machining.
• the density of the sintered compact target was 90.9%, but the bulk resistance exceeded 1 ⁇ 10 3 ⁇ ⁇ cm (1 k ⁇ ⁇ cm). Further, sputtering was performed under the same conditions as in Example 1 using the above-finished 6-inch diameter target, but stable DC sputtering could not be performed.
• the sintered body was finished into a target shape by machining.
• the density of the sintered compact target was 98.7%, but the bulk resistance was a value exceeding 1 ⁇ 10 3 ⁇ ⁇ cm (1 k ⁇ ⁇ cm).
• sputtering was performed under the same conditions as in Example 1 using the above-finished 6-inch diameter target, but stable DC sputtering could not be performed.
• the refractive index (wavelength 550 nm) of the film formation sample was 1.67.
• Example 9 3N equivalent ZnO powder of 5 ⁇ m or less, 3N equivalent of MgO powder with an average particle size of 5 ⁇ m or less, 3N equivalent of Al 2 O 3 powder with an average particle size of 5 ⁇ m or less, 3N equivalent of SiO 2 powder with an average particle size of 5 ⁇ m or less
• 3N which is a low melting point oxide having a melting point of 1000 ° C. or less, and has an average particle size of 5 ⁇ m.
• the following B 2 O 3 powder was prepared at the ratio shown in Table 1. Next, after mixing this, it hot-pressed (HP) at the temperature of 1050 degreeC by argon atmosphere. The pressure of the hot press was 220 kg / cm 2 .
• the sintered body was finished into a target shape by machining.
• the density of the sintered compact target reached 99.2%, and the bulk resistance was 3.0 ⁇ 10 ⁇ 3 ⁇ ⁇ cm (3.0 ⁇ ⁇ cm).
• sputtering was performed under the same conditions as in Example 1 using the above-finished 6-inch ⁇ target. As a result, stable DC sputtering was possible and good sputtering properties were obtained.
• Example 10 ZnO powder of 3N equivalent to 5 ⁇ m or less, 3N equivalent MgO powder with an average particle size of 5 ⁇ m or less, and 3N equivalent Al 2 O 3 powder with an average particle size of 5 ⁇ m or less as a basic raw material, as shown in Table 1, the total amount After adjusting the ratio of the basic raw material so as to be 100 mol%, the ratio shown in Table 1 is the B 2 O 3 powder equivalent to 3N and having an average particle diameter of 5 ⁇ m or less, which is a low melting point oxide having a melting point of 1000 ° C. or less. Prepared with. Next, these powders were prepared in the mixing ratio shown in Table 1, mixed, and then hot pressed (HP) at a temperature of 1050 ° C. in an argon atmosphere. The pressure of the hot press was 220 kg / cm 2 .
• the sintered body was finished into a target shape by machining.
• the density of the sintered compact target reached 99.6%, and the bulk resistance was 2.0 ⁇ 10 ⁇ 3 ⁇ ⁇ cm (3.0 ⁇ ⁇ cm).
• sputtering was performed under the same conditions as in Example 1 using the above-finished 6-inch ⁇ target. As a result, stable DC sputtering was possible and good sputtering properties were obtained.
• Example 11 ZnO powder of 3N equivalent to 5 ⁇ m or less, 3N equivalent of Al 2 O 3 powder with an average particle size of 5 ⁇ m or less, and 3N equivalent of SiO 2 powder with an average particle size of 5 ⁇ m or less as a basic raw material.
• B 2 O 3 powder having an average particle diameter of 5 ⁇ m or less corresponding to 3N which is a low melting point oxide having a melting point of 1000 ° C. or less is shown in Table 1. Formulated in proportions. Next, after mixing this, it hot-pressed (HP) at the temperature of 1050 degreeC by argon atmosphere. The pressure of the hot press was 220 kg / cm 2 .
• the sintered body was finished into a target shape by machining.
• the density of the sintered compact target reached 99.3%, and the bulk resistance was 4.0 ⁇ 10 ⁇ 3 ⁇ ⁇ cm (3.0 ⁇ ⁇ cm).
• sputtering was performed under the same conditions as in Example 1 using the above-finished 6-inch ⁇ target. As a result, stable DC sputtering was possible and good sputtering properties were obtained.
• the feature of the present invention is to achieve low bulk resistance of the sintered body by sintering in an inert gas or vacuum atmosphere even when the component adjustment for lowering the refractive index is performed. This is in that stable DC sputtering is possible. And there is a remarkable effect that the controllability of sputtering, which is the feature of this DC sputtering, can be facilitated, the film forming speed can be increased, and the sputtering efficiency can be improved. In addition, particles (dust generation) and nodules generated during sputtering during film formation can be reduced, and quality variation can be reduced and mass productivity can be improved.
• the sintered compact sputtering target of the present invention is extremely useful for forming thin films such as optical thin films, organic EL televisions, touch panel electrodes, and hard disk seed layers.

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