WO2016088867A1 - Matériau cible de pulvérisation cathodique à base d'oxyde de magnésium et couche mince - Google Patents

Matériau cible de pulvérisation cathodique à base d'oxyde de magnésium et couche mince Download PDF

Info

Publication number
WO2016088867A1
WO2016088867A1 PCT/JP2015/084109 JP2015084109W WO2016088867A1 WO 2016088867 A1 WO2016088867 A1 WO 2016088867A1 JP 2015084109 W JP2015084109 W JP 2015084109W WO 2016088867 A1 WO2016088867 A1 WO 2016088867A1
Authority
WO
WIPO (PCT)
Prior art keywords
mgo
target material
phase
tio
sputtering
Prior art date
Application number
PCT/JP2015/084109
Other languages
English (en)
Japanese (ja)
Inventor
敦志 三谷
真人 財田
寛明 久保
宗佑 横山
Original Assignee
宇部マテリアルズ株式会社
日本タングステン株式会社
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by 宇部マテリアルズ株式会社, 日本タングステン株式会社 filed Critical 宇部マテリアルズ株式会社
Priority to JP2016562691A priority Critical patent/JPWO2016088867A1/ja
Publication of WO2016088867A1 publication Critical patent/WO2016088867A1/fr

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/03—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
    • C04B35/04—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 magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering

Definitions

  • the present invention relates to a sputtering MgO target material and a thin film, and in particular, a sputtering MgO target material mainly composed of Mg (magnesium), Ti (titanium), and O (oxygen), and a thin film formed using the same. It is about.
  • a sputtering method that can easily control the film thickness and components from the angstrom unit to the micron order has been widely used as one of the film formation methods for materials for electronic and electrical parts.
  • a sputtering apparatus having a positive electrode and a negative electrode is used, the substrate and the target material are opposed to each other, and a high voltage is applied between the substrate and the target material in an inert gas atmosphere.
  • the ionized electrons collide with an inert gas to form plasma.
  • the cations in the plasma collide with the surface of the target material (negative electrode) and strike out the target material constituent atoms, and the ejected atoms adhere to the opposing substrate surface to form a film. is there.
  • a target material mainly composed of MgO (magnesium oxide) is used. Since MgO is an insulator, it is usually necessary to use a radio frequency (RF) sputtering method. However, in RF sputtering, an AC voltage is applied between the substrate and the target material. There was a problem of being inferior. Therefore, conventionally, there has been known an MgO target material containing MgO and a conductive material as main components and imparting orientation when deposited by a DC (direct current) sputtering method (see, for example, Patent Document 1). In this document, TiC, VC, WC, and TiN are cited as conductive compounds.
  • a sintered body containing TiO (titanium monoxide) as a main component and added with MgO is also known (for example, see Non-Patent Document 1).
  • This document describes physical properties of a TiO sintered body to which 0 to 20 mol% of MgO is added.
  • MgO is solid-dissolved to 15% in the TiO phase, that the sintered body has a maximum micro Vickers hardness of 1350, an electrical resistivity of 2.8 ⁇ 10 ⁇ 4 ⁇ ⁇ cm, MgO It is described that the relative density decreases with an increase in the amount of added.
  • Non-Patent Document 2 a technique for forming a (Mg 0.2 Ti 0.8 ) O film on a glass substrate by DC sputtering is also known (see, for example, Non-Patent Document 2).
  • Non-Patent Document 2 and Patent Document 2 with a target material composed of Mg, Ti, and O and having a low ratio of Mg to the total amount of Mg and Ti, the crystallinity of the formed alignment film (hereinafter, simply “ In some cases, the crystallinity is low).
  • Patent Document 2 there is a disadvantage that a DC material cannot be formed because a low volume resistivity cannot be obtained when the above-described target material having a high Mg ratio, for example, Mg is 90 mol%.
  • the present invention has an object to provide an MgO target material for sputtering that can be suitably used particularly for DC sputtering, increase the film formation speed, and also has good crystallinity of the alignment film after film formation. To do.
  • Another object of the present invention is to provide a thin film formed using such a sputtering MgO target material.
  • the inventors of the present invention have Mg, Ti, and O as main components as a sputtering target material, and control the ratio of Mg to the total amount of Mg and Ti.
  • the present inventors have found that the volume resistivity of the target material itself is low, DC film formation is possible, and the crystallinity after film formation is good, leading to the present invention.
  • the present invention is an MgO target material for sputtering mainly composed of Mg, Ti, and O, and the ratio of Mg to the total amount of Mg and Ti is in the range of more than 75 and 95 mol% or less, and the volume resistance
  • the present invention relates to an MgO target material for sputtering, wherein the rate is 1 ⁇ 10 2 ⁇ ⁇ cm or less.
  • an MgO phase that is a crystal phase in which Ti and O are the main components and Mg and O are the main components
  • a TiO phase that is a crystal phase in which Ti and O are the main components and Mg is the solid solution.
  • it has a constituent phase containing the MgO phase which has Mg and O as the main ingredients, and the TiO phase which has Ti and O as the main ingredients, and it is preferred that the average particle diameter of the constituent phases is 5 micrometers or less.
  • the relative density is preferably 95% or more.
  • the present invention is a thin film formed using the MgO target material for sputtering described in any of the above.
  • the sputtering MgO target material of the present invention has a low volume resistivity of the target material and a high ratio of Mg, so that the crystallinity of the film after film formation is good.
  • an MgO target material for sputtering that can be suitably used particularly for DC sputtering, increase the film formation speed, and also has good crystallinity of the film after film formation. it can.
  • the sputtering MgO target material of the present invention (hereinafter referred to as “MgO target material”) is a sputtering MgO target (hereinafter referred to as “MgO target”) together with a bonding material such as a backing plate described later.
  • Mg target material a sputtering MgO target (hereinafter referred to as “MgO target”) together with a bonding material such as a backing plate described later.
  • Mg (magnesium), Ti (titanium) and O (oxygen) are the main components, and the ratio of Mg to the total amount of Mg and Ti is more than 75 mol% and not more than 95 mol%.
  • the volume resistivity is 1 ⁇ 10 2 ⁇ ⁇ cm or less.
  • the ratio of Mg to the total amount of Mg and Ti is more than 75 mol% and 95 mol% or less, preferably 80 mol% or more and 95 mol% or less, particularly 90 mol% or more and 95 mol% or less. preferable.
  • the above ratio is 75 mol% or less, the Mg ratio in the thin film formed using the MgO target material becomes low, and the crystallinity of the thin film tends to deteriorate.
  • the above ratio exceeds 95 mol%, the ratio of the MgO phase described later becomes relatively high, and the volume resistivity of the MgO target material tends to be high.
  • the ratio of Mg to the total amount of Mg and Ti can be obtained by composition analysis of the MgO target material.
  • a known analysis method such as an XRF analysis method, an ICP emission analysis method, or a field emission electron beam probe analysis method can be used.
  • the value measured by the method as described in the Example mentioned later is employ
  • the MgO target material can impart orientation to the (002) plane (the same as the (001) plane) on a thin film formed using this MgO target material. Moreover, the thin film after film formation has high crystallinity.
  • the average particle diameter of the constituent phase of the MgO target material is 5 ⁇ m or less, preferably 3 ⁇ m or less, and particularly preferably 1.5 ⁇ m or less.
  • the lower limit of the average particle size of this constituent phase is not particularly limited, but many are limited by the particle size of the raw material powder to be used and the pulverization ability in the process, and therefore it is preferable that it is in a range that can be realized in a normally used process. .
  • the “constituent phase” means all phases constituting the MgO target material, and specifically includes an MgO phase and a TiO phase, which will be described later, in addition to those described later which exist in the MgO target material.
  • a crystalline phase having a structure other than a rock salt structure for example, a spinel phase composed of Mg, Ti, and O
  • an amorphous phase including a single or a plurality of particles filling a region partitioned by these crystalline phases may also be included.
  • the “average particle diameter of the constituent phase” is a minute grain defined by a grain boundary included in a crystal phase constituting the constituent phase (that is, a crystal phase having a structure other than MgO phase, TiO phase, or rock salt structure).
  • grains and an amorphous phase is meant.
  • the MgO target material is a crystal phase mainly composed of Mg and O (hereinafter referred to as “MgO phase”). And a crystal phase mainly composed of Ti and O (hereinafter referred to as “TiO phase”) are mixed. These crystal phases contain a plurality of fine particles defined by grain boundaries.
  • the MgO target material may be in a state where the MgO phase and the TiO phase are completely and uniformly mixed.
  • the MgO phase and the TiO phase basically have a rock salt structure (including a monoclinic structure in which the symmetry of the rock salt structure is reduced).
  • the MgO target material has a crystal phase composed of Mg, Ti and O having a structure other than a rock salt structure (for example, a crystal phase having a spinel structure), a crystal phase mainly composed of Ti and O (for example, A rutile-structured crystal phase), or an amorphous phase composed of a single particle or a plurality of particles filling a region partitioned by these crystal phases.
  • a crystal phase composed of Mg, Ti and O having a structure other than a rock salt structure for example, a crystal phase having a spinel structure
  • a crystal phase mainly composed of Ti and O for example, A rutile-structured crystal phase
  • an amorphous phase composed of a single particle or a plurality of particles filling a region partitioned by these crystal phases.
  • MgO is inherently insulative, but the MgO phase is a crystalline phase containing Mg and O as main components and a small amount of Ti in solid solution, resulting in a decrease in insulation.
  • the TiO phase is a crystalline phase mainly composed of Ti and O and containing a small amount of Mg as a solid solution, and is basically conductive. For this reason, a conductive path is formed in the MgO target material by the crystal particles of the TiO phase contacting each other. Due to the decrease in the insulating properties of the MgO phase, the formation of a conductive path by the TiO phase, and the small average particle size, conductivity capable of DC sputtering can be suitably imparted to the MgO target material.
  • the area of the MgO phase is less than 60% with respect to the whole (that is, the total area of the MgO phase + the area of the TiO phase)
  • the crystallinity of the thin film after film formation tends to be low.
  • the area of the MgO phase exceeds 94% with respect to the whole (the area of the MgO phase + the area of the TiO phase)
  • the overall ratio of the TiO phase becomes too low to form a conductive path, and the MgO target
  • the volume resistivity of the whole material tends to be high.
  • the area of the MgO phase The area of the TiO phase is preferably in the range of 65:35 to 93: 7, more preferably in the range of 70:30 to 92: 8. Note that the image analysis can be performed by a method described in Examples described later.
  • the ratio of the number of Ti atoms to the total number of atoms of Mg and Ti is preferably in the range of 0.05 to 1.00 at% (atomic percent).
  • Ti / Mg + Ti the ratio of the number of Ti atoms to the total number of atoms of Mg and Ti
  • the value of “Ti / Mg + Ti” is less than 0.05 at%, the proportion of Ti contained in the MgO phase decreases, and the volume resistivity of the MgO target material tends to increase.
  • the numerical value of “Ti / Mg + Ti” exceeds 1.00 at%, the proportion of Ti contained in the MgO phase becomes too high and the proportion of the TiO phase relatively decreases, and the volume resistivity of the MgO target material Tends to be higher.
  • the ratio of the number of O atoms to the total number of Mg and Ti atoms is not necessarily 100 at% as long as the MgO target material has the effects of the present invention, for example, by having a rock salt structure. It is not necessary.
  • the ratio of the number of Mg atoms to the total number of Mg and Ti atoms is preferably in the range of 1 to 20 at%.
  • the value of “Mg / Mg + Ti” is less than 1 at%, the ratio of Mg contained in the TiO phase decreases, the ratio of the MgO phase increases relatively, and the volume resistivity of the MgO target material tends to increase.
  • the value of “Mg / Mg + Ti” exceeds 20 at%, the ratio of Mg contained in the TiO phase becomes too high, the resistance of the conductive path is increased, and the volume resistivity of the MgO target material is likely to be increased. .
  • the solid solution amount of atoms in each phase can be calculated by the same method as in the examples described later.
  • the ratio of the number of O atoms to the total number of Mg and Ti atoms is, for example, a rock salt structure or a monoclinic structure in which the symmetry of the rock salt structure is reduced. As long as has the effect of the present invention, it is not necessarily 100 at%.
  • the volume resistivity of the MgO target material is 1 ⁇ 10 2 ⁇ ⁇ cm or less. For this reason, for example, when the film is formed by the DC sputtering method, the discharge can be stably maintained, and the DC sputtering can be performed.
  • the volume resistivity of the MgO target material is preferably 8 ⁇ 10 1 ⁇ ⁇ cm or less, more preferably 5 ⁇ 10 1 ⁇ ⁇ cm or less.
  • the lower limit of the volume resistivity of the MgO target material is not particularly limited, but is preferably lower within the range of ordinary techniques.
  • the relative density of the MgO target material is preferably 95% or more, more preferably 97% or more, and particularly preferably 98% or more. If the relative density of the MgO target material is less than 95%, the MgO target material contains a large number of pores, leading to a decrease in bending strength.
  • the relative density of the MgO target material can be measured by the same method as in the examples described later.
  • the strength of the MgO target material is a three-point bending strength of 250 MPa or more, and more preferably 300 MPa or more. If the three-point bending strength is less than 250 MPa, the MgO target material is likely to break during sputtering film formation, and it is difficult to perform sputtering by applying a large amount of power, so that the film formation rate is suppressed.
  • the bending strength of the MgO target material can be measured by a bending strength test method based on JIS® 1601 (2008 edition).
  • the MgO target material has a low volume resistivity of 1 ⁇ 10 2 ⁇ ⁇ cm or less as described above, it can be suitably formed particularly by a DC sputtering method. For this reason, compared with RF sputtering method, the film-forming speed
  • MgO target material is composed mainly of Mg, Ti and O, and can be manufactured by mixing and sintering magnesium oxide powder and titanium monoxide powder as raw materials. . Each powder is weighed and mixed so that the ratio of Mg to the total amount of Mg and Ti (that is, “Mg / (Mg + Ti)”) is more than 75 mol% and not more than 95 mol%.
  • Mg / (Mg + Ti) magnesium carbonate
  • Mg (OH 2 ) magnesium hydroxide
  • TiH 2 titanium hydride
  • the particle size of the raw material is preferably 1 ⁇ m or less, and may be pulverized to 1 ⁇ m or less during mixing described later.
  • the particle diameter of the raw material is larger than 1 ⁇ m, the average particle diameter of the MgO target material is increased, and as a result, the volume resistivity is increased.
  • a wet ball mill for mixing the raw materials.
  • the solvent an organic solvent such as water or alcohol can be used, and methanol is particularly preferable.
  • the mixing time is not particularly limited, but it is desirable that the mixing time be sufficient for the raw materials to be uniformly mixed. When the raw materials are not uniformly mixed, composition and density unevenness occur in the MgO target material, and the material strength tends to decrease. Further, when mixing the raw materials, a dispersant can be added as necessary.
  • the type of the dispersant is not particularly limited, but is preferably a component that is decomposed by sintering and does not remain.
  • the raw material concentration at the time of mixing is not particularly limited, but generally 15 to 75 wt% is often used with respect to the solvent.
  • the slurry mixed with the raw materials is taken out from the wet ball mill, and the slurry is dried and granulated into a shape suitable for molding.
  • a spray dryer it is preferable to use a spray dryer.
  • a molding aid may be added as necessary.
  • auxiliary agent is not specifically limited, Generally polyvinyl alcohol (PVA), polyethyleneglycol (PEG), cellosol, paraffin, etc. are used.
  • the molding can be performed uniaxially using a mold, CIP (cold isostatic pressing) molding or the like alone or in combination.
  • the molding pressure is not particularly limited, but when a pressure of 100 MPa or more is generally applied, a good molded body can be obtained, which is preferable.
  • the formed body is then subjected to a known sintering method such as magnesium oxide, for example, an atmospheric pressure sintering method, a hot press sintering method, a hot isostatic pressure (HIP) sintering method, a discharge plasma (SPS) sintering method.
  • a known sintering method such as magnesium oxide, for example, an atmospheric pressure sintering method, a hot press sintering method, a hot isostatic pressure (HIP) sintering method, a discharge plasma (SPS) sintering method.
  • Sintering by means of sintering.
  • the sintering temperature is appropriately adjusted depending on the proportion of MgO in the raw material, but is preferably 1000 to 1600 ° C, more preferably 1200 to 1500 ° C. If the sintering temperature is too high, the sintered body will melt, and the desired sintering density and volume resistivity will not be obtained.
  • the sintering pressure is not particularly limited, and may be normal pressure, pressurized or reduced pressure.
  • the sintered body obtained in the above firing step can be used after being processed into a desired shape according to the purpose.
  • a known method such as grinding can be used as a method of the outer shape processing.
  • a sputtering MgO target can be obtained by bonding to a backing plate as required.
  • the thin film of the present invention can be produced by forming a MgO target material by sputtering.
  • the sputtering method the known sputtering method described above can be applied in addition to the DC sputtering method.
  • the sputtering condition is preferably within the range of the substrate temperature of 10 to 500 ° C., particularly preferably within the range of 10 to 300 ° C.
  • the degree of vacuum in the vacuum chamber in which sputtering is performed is preferably 1 ⁇ 10 0 Pa or less.
  • the inside of the vacuum chamber is preferably an inert gas atmosphere such as argon (Ar), helium (He), or nitrogen (N 2 ).
  • the thin film thus obtained becomes an MgO film having a single orientation on the (002) plane.
  • the crystallinity of the thin film is excellent.
  • the MgO film here contains Mg, Ti, and O, and has the same crystal structure as MgO.
  • the thin film of the present invention can be suitably used as an underlayer of a magnetic layer of a magnetic recording medium, for example. Since the magnetic recording medium has a multi-layer structure, when a conventional MgO target material is used, the DC sputtering method and the RF sputtering method have to be properly used depending on the layer. When a material is used, each layer can be manufactured using a DC sputtering method. For this reason, it is possible to increase the manufacturing speed of the magnetic recording medium.
  • the method for measuring the characteristics of the MgO target material and the thin film (sputtered film) is as follows. (1) Measurement of Archimedes density and relative density of MgO target material The sintered density of the MgO target material was measured by the Archimedes method. In addition, the true density in each composition is determined by using a pulverized powder of a target material and a gas pycnometer (Quantachr). ome. The relative density of the MgO target material with respect to the obtained true density was calculated by UPY-2) manufactured by Co.
  • Measurement of relative strength of MgO (002) Measurement of MgO film sputter-deposited on a glass substrate using an MgO target material, using an X-ray diffractometer (manufactured by D8 ADVANCE Bruker AXS), with Out of Plane And the intensity (area) of the MgO (002) peak was calculated.
  • the obtained MgO (002) peak intensity was shown as a relative value with the peak intensity in the MgO target material described in Example 5 described later being 1.
  • SEM Scanning electron microscope
  • Example 1 Preparation of MgO target material and formation and evaluation of sputtered film
  • Example 1 ⁇ Manufacture of MgO target material>
  • Magnesium oxide powder (average particle size 0.2 ⁇ m) and titanium monoxide powder (average particle size 0.15 ⁇ m) are weighed so that MgO is 95 mol% and TiO is 5 mol%.
  • the total weight of magnesium oxide and titanium monoxide was mixed in a resin container containing nylon balls together with 200 parts by weight of a methanol solvent for 100 parts by weight to obtain a raw material slurry.
  • the obtained slurry was dried to obtain granulated powder.
  • the obtained granulated powder is press-molded at a pressure of 100 MPa using a CIP (cold isostatic pressing) molding machine after press molding into a predetermined shape at a surface pressure of 50 MPa using a hydraulic uniaxial molding machine, A compact for a target material was obtained.
  • the obtained compact for target material was fired in an inert gas atmosphere in an electric furnace at a maximum temperature of 1300 ° C. and a holding time of 2 hours to produce an MgO target material.
  • the obtained MgO target material was processed into ⁇ 80 mm ⁇ thickness 4 mm, washed and dried, and then bonded to a backing plate to obtain an MgO target.
  • the obtained MgO target was mounted on a sputtering apparatus (ULVAC CS-L), and was sputter-deposited on a glass substrate (Corning Corporation: EAGLE XG) by a DC magnetron sputtering method, and an MgO film (thickness: 100 nm).
  • the sputtering conditions were as follows: the substrate temperature was 200 ° C., the ultimate vacuum in the chamber was 1 ⁇ 10 ⁇ 4 Pa or less, the Ar gas pressure was 0.2 Pa, and the input power was 100 W.
  • the MgO (002) relative strength of the obtained MgO film was 2.12. The results are shown in Tables 1 and 2.
  • FIG. 1A shows a reflected electron image obtained by SEM observation. From this photograph, it was found that the MgO target material contains an MgO phase (black part) and a TiO phase (white part).
  • Spot 1 of the MgO phase is mainly composed of MgO, and it was found that Ti was dissolved in 0.19% with respect to 99.81% of Mg.
  • Spot 2 of the MgO phase has MgO as the main component, and it was found that 0.16% of Ti was dissolved in 99.84% of Mg.
  • Spot 3 of the TiO phase is mainly composed of TiO, and 6.49% of Mg is dissolved in 93.51% of Ti. That is, it was found that Ti was dissolved in the MgO phase and Mg was dissolved in the TiO phase.
  • Example 2 A MgO target was prepared and a sputtered film was formed and evaluated using the same raw materials and method as in Example 1 except that MgO was 92 mol% and TiO was 8 mol%. The results are shown in Tables 1 and 2. Further, the average particle size was measured by the method of “(9) Measurement of average particle size of constituent phases constituting target material”. As a result, the average particle size was 1.5 ⁇ m. The results are shown in Table 5.
  • Example 3 Except that MgO was changed to 90 mol% and TiO was changed to 10 mol%, an MgO target was prepared and a sputtered film was formed and evaluated using the same raw materials and methods as in Example 1. The results are shown in Tables 1 and 2.
  • Example 4 A MgO target was prepared and a sputtered film was formed and evaluated using the same raw materials and method as in Example 1 except that MgO was 80 mol% and TiO was 20 mol%. The results are shown in Tables 1 and 2.
  • Example 2 Further, TEM observation was performed in the same manner as in Example 1. The obtained backscattered electron image is shown in FIG. Moreover, the area ratio of MgO phase and TiO phase and the amount of solid solution in each phase were calculated. The results are shown in Table 3 and Table 4, respectively.
  • Example 5 A MgO target was prepared and a sputtered film was formed and evaluated using the same raw materials and method as in Example 1 except that 77 mol% of MgO and 23 mol% of TiO were used. The results are shown in Tables 1 and 2.
  • Example 6 As in Example 2, MgO was 92 mol%, TiO was 8 mol%, the particle diameter of MgO powder was 0.5 ⁇ m, and the particle diameter of TiO powder was 0.7 ⁇ m.
  • the target material was manufactured. The average particle diameter and volume resistivity were measured in the same manner as in Example 2. The results are shown in Table 5.
  • Example 7 An MgO target material was produced in the same manner as in Example 6 except that the particle diameter of the MgO powder was 0.2 ⁇ m and the particle diameter of the TiO powder was 0.3 ⁇ m. The average particle diameter and volume resistivity were measured in the same manner as in Example 2. The results are shown in Table 5.
  • Example 8 An MgO target material was produced in the same manner as in Example 6 except that the particle diameter of the MgO powder was 0.1 ⁇ m and the particle diameter of the TiO powder was 0.08 ⁇ m. The average particle diameter and volume resistivity were measured in the same manner as in Example 2. The results are shown in Table 5.
  • Example 1 A MgO target was prepared and a sputtered film was formed and evaluated in the same manner as in Example 1 except that MgO was changed to 100 mol%. Since the resistance value of the MgO target material was too high, the volume resistivity could not be measured. Further, since the MgO target material had high resistance and could not be formed, the MgO (002) relative strength could not be evaluated. The results are shown in Tables 1 and 2.
  • Example 2 A MgO target was prepared and a sputtered film was formed and evaluated in the same manner as in Example 1 except that MgO was changed to 98 mol% and TiO was changed to 2 mol%. Further, since the MgO target material had high resistance and could not be formed, the MgO (002) relative strength could not be evaluated. The results are shown in Tables 1 and 2.
  • Example 3 A MgO target was prepared and a sputtered film was formed and evaluated in the same manner as in Example 1 except that MgO was 75 mol% and TiO was 25 mol%. The results are shown in Tables 1 and 2.
  • Example 4 A MgO target was prepared and a sputtered film was formed and evaluated in the same manner as in Example 1 except that MgO was 70 mol% and TiO was 30 mol%. The results are shown in Tables 1 and 2.
  • Example 5 A MgO target was prepared and a sputtered film was formed and evaluated in the same manner as in Example 1 except that MgO was 50 mol% and TiO was 50 mol%. The results are shown in Tables 1 and 2.
  • Example 6 An MgO target material was produced in the same manner as in Example 1 except that MgO was 92 mol%, TiO was 8 mol%, the particle diameter of MgO powder was 1 ⁇ m, and the particle diameter of TiO powder was 1 ⁇ m. The average particle diameter and volume resistivity were measured in the same manner as in Example 2. The results are shown in Table 5.
  • FIG. 2 shows the volume resistivity ( ⁇ plot) of the examples of the present application, comparative examples (both TiO), and the volume resistivity ( ⁇ of the example containing TiC among the MgO target materials described in the examples of Patent Document 1. It is a graph in which the volume resistivity ( ⁇ plot) of an example including TiN is overlaid and plotted.

Abstract

Cette invention concerne un matériau cible de pulvérisation cathodique à base de MgO, comprenant du Mg, du Ti et de l'O en tant que composants principaux, le matériau cible de pulvérisation cathodique à base de MgO étant caractérisé en ce que le pourcentage de Mg par rapport à la quantité totale de Mg et de Ti est dans une plage allant de plus de 75 à 95 % en moles et sa résistivité en volume est inférieure ou égale à 1 × 102 Ω·cm. De préférence, le matériau cible de pulvérisation cathodique à base de MgO comprend : une phase de MgO qui contient du Mg et de l'O en tant que composants principaux et qui continent du Ti en tant que soluté en solution solide; et une phase de TiO qui contient du Ti et de l'O en tant que composants principaux et qui contient du Mg en tant que soluté en solution solide. L'invention concerne également une couche mince caractérisée en ce que la couche est formée au moyen dudit matériau cible de pulvérisation cathodique à base de MgO.
PCT/JP2015/084109 2014-12-05 2015-12-04 Matériau cible de pulvérisation cathodique à base d'oxyde de magnésium et couche mince WO2016088867A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2016562691A JPWO2016088867A1 (ja) 2014-12-05 2015-12-04 スパッタリング用ＭｇＯターゲット材及び薄膜

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2014247028 2014-12-05
JP2014-247028 2014-12-05

Publications (1)

Publication Number Publication Date
WO2016088867A1 true WO2016088867A1 (fr) 2016-06-09

Family

ID=56091806

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2015/084109 WO2016088867A1 (fr) 2014-12-05 2015-12-04 Matériau cible de pulvérisation cathodique à base d'oxyde de magnésium et couche mince

Country Status (3)

Country Link
JP (1) JPWO2016088867A1 (fr)
TW (1) TW201632482A (fr)
WO (1) WO2016088867A1 (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2019019402A (ja) * 2017-07-21 2019-02-07 Ｊｘ金属株式会社 スパッタリングターゲット、スパッタリングターゲットの製造方法及び磁気媒体の製造方法
JP2020147822A (ja) * 2019-03-15 2020-09-17 株式会社高純度化学研究所 ＭｇＯ−ＴｉＯ系スパッタリングターゲットの製造方法
JP2020164959A (ja) * 2019-03-29 2020-10-08 Ｊｘ金属株式会社 スパッタリングターゲット部材、スパッタリングターゲット、スパッタリングターゲット部材の製造方法、及びスパッタ膜の製造方法
CN113661143A (zh) * 2019-07-23 2021-11-16 松下知识产权经营株式会社 薄膜的制造方法以及层叠体
CN115246732A (zh) * 2021-04-28 2022-10-28 光洋应用材料科技股份有限公司 复合氧化物靶材及其制法
JP7165787B1 (ja) 2021-04-26 2022-11-04 光洋應用材料科技股▲分▼有限公司 複合酸化物ターゲット及びその製造方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH085708B2 (ja) * 1987-10-01 1996-01-24 東芝タンガロイ株式会社 酸化物系セラミックス
JP2013241684A (ja) * 2011-07-01 2013-12-05 Ube Material Industries Ltd スパッタリング用ＭｇＯターゲット
WO2014156497A1 (fr) * 2013-03-29 2014-10-02 Jx日鉱日石金属株式会社 Cible comprimée frittée en mgo-tio et son procédé de production

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH085708B2 (ja) * 1987-10-01 1996-01-24 東芝タンガロイ株式会社 酸化物系セラミックス
JP2013241684A (ja) * 2011-07-01 2013-12-05 Ube Material Industries Ltd スパッタリング用ＭｇＯターゲット
WO2014156497A1 (fr) * 2013-03-29 2014-10-02 Jx日鉱日石金属株式会社 Cible comprimée frittée en mgo-tio et son procédé de production

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2019019402A (ja) * 2017-07-21 2019-02-07 Ｊｘ金属株式会社 スパッタリングターゲット、スパッタリングターゲットの製造方法及び磁気媒体の製造方法
JP7014541B2 (ja) 2017-07-21 2022-02-01 Ｊｘ金属株式会社 スパッタリングターゲット、スパッタリングターゲットの製造方法及び磁気媒体の製造方法
JP2020147822A (ja) * 2019-03-15 2020-09-17 株式会社高純度化学研究所 ＭｇＯ−ＴｉＯ系スパッタリングターゲットの製造方法
JP7178707B2 (ja) 2019-03-15 2022-11-28 株式会社高純度化学研究所 ＭｇＯ－ＴｉＯ系スパッタリングターゲットの製造方法
JP2020164959A (ja) * 2019-03-29 2020-10-08 Ｊｘ金属株式会社 スパッタリングターゲット部材、スパッタリングターゲット、スパッタリングターゲット部材の製造方法、及びスパッタ膜の製造方法
WO2020202649A1 (fr) * 2019-03-29 2020-10-08 Ｊｘ金属株式会社 Élément de cible de pulvérisation cathodique, cible de pulvérisation cathodique, procédé de production d'un élément de cible de pulvérisation cathodique et procédé de production de film de pulvérisation cathodique
JP7246232B2 (ja) 2019-03-29 2023-03-27 Ｊｘ金属株式会社 スパッタリングターゲット部材、スパッタリングターゲット、スパッタリングターゲット部材の製造方法、及びスパッタ膜の製造方法
CN113661143A (zh) * 2019-07-23 2021-11-16 松下知识产权经营株式会社 薄膜的制造方法以及层叠体
CN113661143B (zh) * 2019-07-23 2024-03-08 松下知识产权经营株式会社 薄膜的制造方法以及层叠体
JP7165787B1 (ja) 2021-04-26 2022-11-04 光洋應用材料科技股▲分▼有限公司 複合酸化物ターゲット及びその製造方法
JP2022172036A (ja) * 2021-04-26 2022-11-14 光洋應用材料科技股▲分▼有限公司 複合酸化物ターゲット及びその製造方法
CN115246732A (zh) * 2021-04-28 2022-10-28 光洋应用材料科技股份有限公司 复合氧化物靶材及其制法

Also Published As

Publication number Publication date
TW201632482A (zh) 2016-09-16
JPWO2016088867A1 (ja) 2017-09-21

Similar Documents

Publication Publication Date Title
WO2016088867A1 (fr) Matériau cible de pulvérisation cathodique à base d'oxyde de magnésium et couche mince
KR101731847B1 (ko) 스퍼터링용 MgO 타겟
TWI616425B (zh) MgO-TiO sintered body target and manufacturing method thereof
JP5887819B2 (ja) 酸化亜鉛焼結体、それから成るスパッタリングターゲットおよび酸化亜鉛薄膜
KR20120120127A (ko) Ｓｂ-Ｔｅ기 합금 소결체 스퍼터링 타깃
JPWO2004079036A1 (ja) スパッタリングターゲット及びその製造方法
JP2010208871A (ja) 酸化アルミニウム焼結体、その製法及び半導体製造装置部材
JP6052976B2 (ja) 静電チャック誘電体層および静電チャック
JP2007290875A (ja) 酸化チタン系焼結体およびその製造方法
JPWO2019163710A1 (ja) 複合焼結体、半導体製造装置部材および複合焼結体の製造方法
JP6537715B2 (ja) Ａｌ２Ｏ３スパッタリングターゲット及びその製造方法
JP7108046B2 (ja) 酸化マグネシウムスパッタリングターゲット
JP6149804B2 (ja) 酸化物焼結体及びその製造方法
CN112236403B (zh) 靶和用于制造靶的方法
WO2012073879A1 (fr) Cible de pulvérisation
JP6635862B2 (ja) ＢｉＦｅＯ３系焼結体からなるスパッタリングターゲット及びその製造方法
JP6459830B2 (ja) 酸化物焼結体及びその製造方法、並びに酸化物膜の製造方法
WO2019177086A1 (fr) CORPS FRITTÉ EN MgO ET CIBLE DE PULVÉRISATION
JP7178707B2 (ja) ＭｇＯ－ＴｉＯ系スパッタリングターゲットの製造方法
JP7165023B2 (ja) 酸化マグネシウムスパッタリングターゲット
US20220285164A1 (en) Plasma Etching Apparatus Component for Manufacturing Semiconductor Comprising Composite Sintered Body and Manufacturing Method Therefor
JP2009004752A (ja) 静電チャック
JP2015227262A (ja) 酸化物焼結体及びその製造方法、並びに酸化物膜

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 15866122

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 2016562691

Country of ref document: JP

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 15866122

Country of ref document: EP

Kind code of ref document: A1