WO2014178310A1 - Corps fritté, et cible de pulvérisation pour utilisation dans la formation de film d'enregistrement magnétique qui comprend ledit corps fritté - Google Patents

Corps fritté, et cible de pulvérisation pour utilisation dans la formation de film d'enregistrement magnétique qui comprend ledit corps fritté Download PDF

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Publication number
WO2014178310A1
WO2014178310A1 PCT/JP2014/061357 JP2014061357W WO2014178310A1 WO 2014178310 A1 WO2014178310 A1 WO 2014178310A1 JP 2014061357 W JP2014061357 W JP 2014061357W WO 2014178310 A1 WO2014178310 A1 WO 2014178310A1
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Prior art keywords
sintered body
oxide
mol
boron
body according
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PCT/JP2014/061357
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English (en)
Japanese (ja)
Inventor
英生 高見
中村　祐一郎
祐希 池田
真一 荻野
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Jx日鉱日石金属株式会社
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Application filed by Jx日鉱日石金属株式会社 filed Critical Jx日鉱日石金属株式会社
Priority to SG11201506155PA priority Critical patent/SG11201506155PA/en
Priority to JP2014541456A priority patent/JP5878242B2/ja
Priority to CN201480011201.XA priority patent/CN105026589B/zh
Publication of WO2014178310A1 publication Critical patent/WO2014178310A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only 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
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/07—Alloys based on nickel or cobalt based on cobalt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/04—Alloys based on a platinum group metal

Definitions

  • the present invention relates to a sintered body, which is useful for forming a magnetic thin film of a magnetic recording medium, particularly a magnetic recording film used for forming a magnetic recording layer of a hard disk adopting a perpendicular magnetic recording system
  • the present invention relates to a sputtering target made of the sintered body.
  • a target prepared from a sintered body containing boron oxide particles of boron oxide are coarsened during or after sintering, so that many particles are generated during sputtering.
  • This invention relates to the sputtering target which consists of a sintered compact which can solve such a problem, and the sintered compact.
  • a material based on Co, Fe, or Ni which is a ferromagnetic metal, is used as a magnetic thin film material for recording.
  • a Co—Cr-based or Co—Cr—Pt-based ferromagnetic alloy containing Co as a main component has been used for a recording layer of a hard disk employing an in-plane magnetic recording method.
  • a composite material composed of a Co—Cr—Pt ferromagnetic alloy containing Co as a main component and a non-magnetic inorganic material is often used for a recording layer of a hard disk employing a perpendicular magnetic recording method that has been put into practical use in recent years. ing.
  • a magnetic thin film of a magnetic recording medium such as a hard disk is often produced by sputtering a ferromagnetic material sputtering target containing the above material as a component because of high productivity. Further, boron oxide is added to such a sputtering target for a magnetic recording film in order to magnetically separate the alloy phase.
  • a melting method or a powder metallurgy method can be considered as a method for producing a ferromagnetic material sputtering target. Which method is used depends on the required characteristics, so it cannot be generally stated, but the sputtering target made of a ferromagnetic alloy and non-magnetic inorganic particles used for the recording layer of a perpendicular magnetic recording hard disk is Generally, it is produced by a powder metallurgy method. This is because inorganic particles such as boron oxide need to be uniformly dispersed in the alloy substrate, and thus it is difficult to produce by the melting method.
  • Patent Document 1 states that “a magnetic recording medium having a magnetic data recording layer, wherein the magnetic data recording layer has a magnetic difference of at least 0.5 ⁇ 10 7 erg / cm 3 (0.5 / Jcm 3 ).
  • a magnetic recording medium comprising: a first alloy having an isotropic constant; and an oxide compound comprising oxygen and one or more elements in which at least one element has a negative reduction potential. 1) is described.
  • “at least one of the one or more elements in the oxide compound is lithium (Li), beryllium (Be), boron (B), sodium (Na), magnesium.
  • Mg aluminum (Al), silicon (Si), potassium (K), calcium (Ca), scandium (Sc), titanium (Ti), vanadium (V), chromium (Cr), manganese (Mn), iron (Fe), cobalt (Co), nickel (Ni), zinc (Zn), gallium (Ga), rubidium (Rb), strontium (Sr), yttrium (Y), zirconium (Zr), niobium (Nb), cadmium (Cd), indium (In), cesium (Cs), barium (Ba), lanthanum (La), cerium (Ce), praseodymium (Pr), neo (Nd), samarium (Sm), europium (Eu), terbium (Tb), gadolinium (
  • Claim 1 of the following Patent Document 2 states that “a target used for forming a Co-based magnetic layer of a magnetic recording medium by a sputtering method, wherein the target contains 5 mol% or more of Cr or Cr alloy, and contains CoO.
  • the oxide having a melting point of 800 ° C. or lower is at least one selected from boron oxide, vanadium oxide, tellurium oxide, molybdenum oxide, and low-melting glass.
  • “Target described in item 1" is described. In this case as well, there is no description about the problem of the presence of boron oxide in the sintered body or the target made of the sintered body and the solution to the problem, as in the case of the above-mentioned document 1.
  • Patent Document 3 listed below is a sintered sputtering target made of a ferromagnetic alloy having a Cr content of 20 mol% or less and the balance being Co and a non-metallic inorganic material, and the volume ratio occupied by the non-metallic inorganic material is 40 vol% or less.
  • the sputtering target is characterized in that the non-metallic inorganic material contains at least cobalt oxide and boron oxide.
  • Sputtering which forms and sinters the mixed powder obtained by pulverizing and mixing the metal powder and the non-metallic inorganic material powder containing at least cobalt oxide and boron oxide at a holding temperature of 800 ° C or less.
  • Patent Document 4 describes “a sputtering target for a magnetic recording film containing SiO 2 and containing 10 to 1000 wtppm of B (boron)”. Yes. In this case, boron oxide is also included. However, as in the above-mentioned documents 1, 2, and 3, the problem of the presence of boron oxide in the sintered body or the target composed of the sintered body, and the solution of the problem There is no mention of any method.
  • a composite material composed of a ferromagnetic alloy and a nonmagnetic material is often used, and boron oxide is added as a nonmagnetic material.
  • boron oxide particles become large after sintering. Therefore, if the sintering temperature is lowered in order to suppress grain growth, the density cannot be increased and many particles are generated. It was.
  • boron oxide raw materials are highly hygroscopic and easily solidify, making it difficult to obtain fine boron oxide.
  • the sintered body in which the boron oxide remains when wet-processed by machining or stored in a place with high humidity, it reacts with moisture to generate boric acid, which is baked. It precipitates on the surface of the bonded body (target) and causes stains and dirt, which also causes generation of particles during sputtering, and moisture is taken into the film and causes defects. It was. In order to ensure good quality of a sintered body for forming a magnetic recording film to which boron oxide is added, particularly a sputtering target, it is necessary to solve such a problem.
  • the present invention 1) A sintered body comprising at least one metal selected from the group consisting of cobalt and one or more metals or alloys selected from boron and / or platinum group elements, and an oxide, wherein the phase comprising the oxide is Cr
  • a sintered body characterized in that at least one of (BO 3 ), Co 2 B 2 O 5 , and Co 3 B 2 O 6 is present.
  • the present invention also provides: 2) A sintered body comprising at least cobalt as a metal, chromium, one or more metals or alloys selected from boron and / or platinum group elements, and an oxide, the phase comprising the oxide And a sintered body characterized in that at least one of Cr (BO 3 ), Co 2 B 2 O 5 , and Co 3 B 2 O 6 is present.
  • the present invention also provides: 3) The sintered body according to any one of 1) or 2) above, wherein the sintered body has no discoloration when contacted or immersed in water. .
  • the present invention also provides: 4) The sintered body according to any one of 2) or 3) above, wherein the atomic ratio of chromium to boron is Cr / B ⁇ 1.
  • the present invention also provides: 5) The sintered body according to any one of 1) to 4) above, wherein the atomic ratio of boron to oxygen is B / O ⁇ 0.5.
  • the present invention also provides: 6) The ratio of the metal component is such that the chromium content is 0 to 50 mol%, the boron and / or platinum group element content is 0 (excluding 0) to 40 mol%, and the balance is cobalt.
  • the sintered body according to any one of 1) to 5) above is provided.
  • the present invention also provides: 7) The sintered body according to any one of 1) to 6) above, wherein the boron oxide content is 0.5 to 10 mol% in terms of B 2 O 3 .
  • the present invention also provides: 8) The sintered body according to any one of 1) to 7) above, wherein the total content of chromium oxide is 0.5 to 10 mol% in terms of Cr 2 O 3 .
  • the present invention also provides: 9) Further, Al, Co, Cu, Fe, Ga, Ge, Hf, Li, Mg, Mn, Mo, Nb, Ni, Sb, Si, Sn, Ta, Te, Ti, V, W, Y, Zn or Zr
  • a sintered body is any one of 1) to 8) above, wherein an oxide containing at least one element selected from the group consisting of 2 to 8 wt% in terms of oxygen is contained.
  • the present invention also provides: 10) The sintered body according to any one of 1) to 9) above, wherein the average area per one particle of the oxide in the sintered body is 2 ⁇ m 2 or less.
  • the present invention also provides: 11) The sintered body according to any one of 1) to 10) described above further includes 0.5 mol% or more of at least one element selected from Ti, V, Mn, Zr, Nb, Mo, Ta, and W. A sintered body containing 10 mol% or less is provided.
  • the present invention also provides: 12) The sintered body according to any one of 1) to 11) above, further comprising at least one selected from carbon, nitride, and carbide.
  • the present invention also provides: 13) The sintered body according to any one of 1) to 12) above, wherein the relative density is 95% or more.
  • the present invention also provides: 14) Provided is a sputtering target for forming a magnetic recording film comprising the sintered body according to any one of 1) to 13) above.
  • the present invention also provides: 15) At least one of one or more metals or alloys selected from boron and / or platinum group elements, and at least one of Cr (BO 3 ), Co 2 B 2 O 5 , and Co 3 B 2 O 6 , including at least cobalt as a metal.
  • a method for producing a sintered body characterized by mixing and sintering seeds or more oxides.
  • the present invention also provides: 16) At least cobalt as a metal, one or more metals or alloys selected from chromium, boron and / or platinum group elements, Cr (BO 3 ), Co 2 B 2 O 5 , Co 3 B 2 O 6 There is provided a method for producing a sintered body comprising mixing and sintering at least one kind of oxide.
  • the present invention also provides: 17) Boron oxide and chromium oxide and / or cobalt oxide are prepared, and this is fired in the atmosphere, and at least one of Cr (BO 3 ), Co 2 B 2 O 5 , and Co 3 B 2 O 6
  • the present invention also provides: 18) The sintered body according to any one of 1) to 13) above is manufactured by the method for manufacturing a sintered body according to any one of 15) to 17) above. A method for producing a sintered body is provided.
  • the sintered body to which boron oxide is added has a problem that particles of boron oxide become large after sintering, and many particles are generated when used as a sputtering target for forming a magnetic recording film. .
  • the cause is that boron oxide raw material is highly hygroscopic and solidifies easily, so it is difficult to obtain fine boron oxide.
  • boron oxide has a low melting point, it easily liquefies during sintering, It grows into large particles.
  • At least one of Cr (BO 3 ), Co 2 B 2 O 5 , and Co 3 B 2 O 6 is included in the phase of the oxide in the sintered body of the present invention, in particular, the sputtering target for a magnetic recording film.
  • Cr (BO 3 ), Co 2 B 2 O 5 , and Co 3 B 2 O 6 can maintain a fine structure, increase the melting point of boron oxide, and suppress reaction with water. It has the characteristics that can be. As a result, it has become possible to solve the above-mentioned problems caused by boron oxide in the sintered body.
  • the sintered body of the present invention particularly a sputtering target for a magnetic recording film, includes cobalt as a metal, one or more metals or alloys selected from chromium and platinum group elements, and an oxide containing boron oxide and chromium oxide. It is a sintered body, particularly a sputtering target for a magnetic recording film. In addition to this (other than the above component composition), other metal materials and inorganic materials described later can be further added.
  • the “one or more metals or alloys selected from chromium and platinum group elements” may be chromium metal alone, one or more metals selected from platinum group elements, or these It means that an alloy may be used.
  • the sintered body of the present invention is mainly used as a sputtering target. In that sense, the following will be described mainly with respect to the sputtering target of the main application, but this sintered body is not prevented from being used as another coating (coating) method. For example, it can be used for physical and chemical vapor deposition such as ion beam vapor deposition.
  • the sintered body of the present invention includes these.
  • the present invention requires that at least one of Cr (BO 3 ), Co 2 B 2 O 5 , and Co 3 B 2 O 6 is present in the phase comprising the oxide, and this is a requirement of the present application.
  • This is one of the major features of the invention.
  • boron oxide exists in the form of the compound as described above, it has characteristics and effects that can maintain a fine structure, increase the melting point of boron oxide, and suppress reaction with water. Can do.
  • the atomic ratio of chromium and boron is preferably Cr / B ⁇ 1. This is confirmed by an experiment, and when it is out of this range, it easily reacts with water. Although other ranges can be used, this atomic ratio can be said to be a more preferable range.
  • the atomic ratio of boron and oxygen is B / O ⁇ 0.5. This is confirmed by an experiment, and when it is out of this range, it easily reacts with water. Although other ranges can be used, this atomic ratio can be said to be a more preferable range.
  • the sintered body of the present invention can be applied to a general magnetic material target.
  • the chromium content is 0 to 50 mol%.
  • the content of boron and / or platinum group elements is 0 (excluding 0) to 40 mol%, and the balance is cobalt.
  • it may be a chromium metal alone, one or more metals selected from boron and / or platinum group elements, or an alloy thereof.
  • inclusion of boron oxide in the above form is an important point of the invention, it can be said that it is not necessary to be limited to the above composition range, but as a basic composition of a suitable magnetic material, The above can be mentioned.
  • the boron oxide content (also referred to as the addition amount) can be applied to 0.5 to 10 mol% in terms of B 2 O 3 .
  • boron contained as a component exists as a compound of at least Cr (BO 3 ), Co 2 B 2 O 5 , or Co 3 B 2 O 6 .
  • the total content of chromium oxide is preferably 0.5 to 10 mol% in terms of Cr 2 O 3 . This also shows a preferable range as a sputtering target for a magnetic recording film.
  • An oxide containing one or more elements selected from Y, Zn, and Zr is included, and the total oxide amount is 2 to 8 wt% in terms of oxygen.
  • These also show a suitable range as a sintered body, particularly as a sputtering target for a magnetic recording film.
  • the addition of these oxides is not particularly shown in the examples, it is a suitable material generally added to the magnetic recording film, and can be similarly applied to the present invention.
  • the average area per one particle of the oxide phase is desirably 2 ⁇ m 2 or less.
  • an oxide phase can be observed, and it is desirable that the oxide phase is finely dispersed. This is because if there is a coarse oxide phase, arcing or particles are easily generated during sputtering.
  • said area shows the suitable range as a sputtering target for magnetic recording films, and use of what exceeds these ranges is not prevented by the relation with the purpose of use or other materials.
  • the sintered body of the present invention described above, particularly the sputtering target for a magnetic recording film, is additionally selected from Ti, V, Mn, Zr, Nb, Mo, Ta, and W as a single additive element. More than element and 0.5 mol% or more and 10 mol% or less can be contained. These additive elements are added as necessary in order to improve the characteristics as a magnetic recording medium. These additive elements are not particularly shown in the examples, but are suitable materials generally added to the magnetic recording film, and can be similarly applied to the present invention.
  • an inorganic material having one or more components selected from carbon, nitride, and carbide can be contained as an additive material. These are elements that are added as necessary in order to improve the characteristics as a magnetic recording medium.
  • the sintered body of the present invention having the above component composition, particularly a sputtering target for a magnetic recording film, a relative density of 95% or more, 98% or more, and 99% or more can be achieved.
  • the density of the sintered body can be adjusted by the sintering temperature and the pressure of the hot press or HIP. However, if the temperature is too high, the oxide phase grows and coarsens, so the sintering temperature is lowered as much as possible to increase the pressure. It is desirable to do.
  • the sintering temperature is desirably 1100 ° C. or lower and the pressure is preferably 250 kgf / cm 2 or higher. Molding / sintering is not limited to hot pressing, and plasma discharge sintering and hot isostatic pressing can also be used.
  • the relative density is a value obtained by dividing the actually measured density of the target by the calculated density (also called the theoretical density).
  • the calculation density is a density when it is assumed that the constituent components of the target are mixed without diffusing or reacting with each other, and is calculated by the following equation.
  • Calculated density Sigma ⁇ (Molecular weight of constituent component x Molar ratio of constituent component) / ⁇ (Molecular weight of constituent component x Molar ratio of constituent component / Document value density of constituent component)
  • ⁇ means taking the sum for all the constituent components of the target.
  • the sintered body of the component composition range specified in the present invention particularly the sputtering target for magnetic recording film, It has the same effect as.
  • the sintering raw material at least one metal containing cobalt as a metal and selected from chromium and platinum group elements, and further necessary raw material powders of oxides in the ratios shown in Table 1.
  • a graphite die having a diameter of 50 ⁇ and subjected to hot press sintering at a sintering temperature of 900 to 1100 ° C. in vacuum.
  • a sintering temperature of 900 to 1100 ° C. in vacuum.
  • it was immersed in pure water for 1 hour at room temperature and then dried to observe the surface.
  • the production method and test method were the same as those in this example.
  • Each component composition of the magnetic material used as the matrix in Example 1 was Co: 69 mol%, Cr: 5 mol%, and Pt: 20 mol%.
  • the oxides were Cr (BO 3 ): 2 mol%, Cr 2 O 3 : 2 mol%, and SiO 2 : 2 mol%.
  • the ratio of Cr / B is 5.5.
  • the B / O ratio was 0.1.
  • the results are shown in Table 1.
  • the average area per one particle of the oxide phase in the target was 1.5 ⁇ m 2 .
  • grains of an oxide phase is calculated
  • sputtering was performed by producing a target from a 180 ⁇ size sintered body produced with the same raw materials and production conditions, the number of particles generated in a steady state was 2, and thus a high-density target was obtained. The number of particles generated was small.
  • Example 2 A sintered body was produced under the same conditions as in Example 1 except that each component composition was adjusted to Table 1.
  • Each component composition of the magnetic material used as the matrix of Example 2 was set to Co: 60 mol%, Cr: 5 mol%, Pt: 20 mol%, Ru: 5 mol%.
  • the oxide was Cr (BO 3 ): 10 mol%.
  • the ratio of Cr / B is 1.5.
  • the B / O ratio was 0.3.
  • the results are also shown in Table 1.
  • the average area per one particle of the oxide phase in the target was 1.9 ⁇ m 2 .
  • the appearance of the surface of the sintered body after being immersed in water had no discoloration.
  • the relative density of this sintered compact was 95.8%.
  • Example 3 A sintered body was produced under the same conditions as in Example 1 except that each component composition was adjusted to Table 1.
  • Each component composition of the magnetic material used as the matrix of Example 3 was Co: 77.8 mol%, Cr: 5.3 mol%, and Pt: 10.5 mol%.
  • the oxides were Cr (BO 3 ): 4.2 mol%, Co 2 B 2 O 5 : 1.1, and Co 3 B 2 O 6 : 1.1.
  • the ratio of Cr / B is 1.7.
  • the B / O ratio was 0.3.
  • the results are also shown in Table 1.
  • the average area per particle of the oxide phase in the target was 1.1 ⁇ m 2 .
  • the appearance of the surface of the sintered body after being immersed in water had no discoloration.
  • the relative density of this sintered body was 96.1%.
  • Example 4 A sintered body was produced under the same conditions as in Example 1 except that each component composition was adjusted to Table 1.
  • Each component composition of the magnetic material used as the matrix of Example 4 was set to Co: 75.2 mol% and Pt: 21.5 mol%.
  • the oxides were Co 2 B 2 O 5 : 2.2 and Co 3 B 2 O 6 : 1.1.
  • the ratio of Cr / B is 0.0.
  • the B / O ratio was 0.4. These satisfied the conditions of the present invention.
  • the results are also shown in Table 1.
  • the average area per one particle of the oxide phase in the target was 2.0 ⁇ m 2 .
  • the appearance of the surface of the sintered body after being immersed in water had no discoloration.
  • the relative density of this sintered body was 97.1%.
  • Example 5 A sintered body was produced under the same conditions as in Example 1 except that each component composition was adjusted to Table 1.
  • the composition of each component of the magnetic material serving as the matrix of Example 5 was Co: 71.4 mol% and Pt: 20.4 mol%.
  • the oxides were Cr (BO 3 ): 4.1 mol%, Co 2 B 2 O 5 : 1, TiO 2 : 3.1 mol%.
  • the ratio of Cr / B is 0.7.
  • the B / O ratio was 0.3. Except for the Cr / B ratio, the conditions of the present invention were satisfied.
  • the results are also shown in Table 1.
  • the average area per particle of the oxide phase in the target was 1.2 ⁇ m 2 .
  • the appearance of the surface of the sintered body after being immersed in water had no discoloration.
  • the relative density of this sintered body was 97.5%.
  • Example 6 A sintered body was produced under the same conditions as in Example 1 except that each component composition was adjusted to Table 1.
  • the composition of each component of the magnetic material serving as the matrix of Example 6 was Co: 55 mol%, Cr: 30 mol%, and Ru: 5 mol%. Meanwhile, oxides, Cr (BO 3): 2mol %, TiO 2: was a 8 mol%.
  • the ratio of Cr / B is 16. The B / O ratio was 0.09. All satisfied the conditions of the present invention.
  • the results are also shown in Table 1.
  • the average area per one particle of the oxide phase in the target was 1.9 ⁇ m 2 .
  • the appearance of the surface of the sintered body after being immersed in water had no discoloration.
  • the relative density of this sintered body was 99.5%.
  • Example 7 A sintered body was produced under the same conditions as in Example 1 except that each component composition was adjusted to Table 1.
  • Each component composition of the magnetic material used as the matrix of Example 7 was set to Co: 55 mol%, Cr: 30 mol%, and B: 5 mol%. Meanwhile, oxides, CoO: 6mol%, TiO 2 : was 4 mol%.
  • the ratio of Cr / B is 6.
  • the B / O ratio was 0.36. All satisfied the conditions of the present invention. After sintering, it was confirmed that a part of Cr (BO 3 ) was produced by XRD measurement of the sample.
  • the XRD measurement conditions were using Rigaku's Ultimate IV, using CuK ⁇ rays, tube voltage 40 kv, tube current 30 mA, scan speed 1 ° / min, step 0.01 °, and scan angle range (2 ⁇ ) of 24 to 35. °.
  • the intensity of the first peak was 120 cps
  • the intensity of the second peak was 70 cps (the background intensity was approximately 50 cps).
  • strength values are fluctuate
  • the results are also shown in Table 1.
  • the average area per one particle of the oxide phase in the target was 1.9 ⁇ m 2 .
  • the appearance of the surface of the sintered body after being immersed in water had no discoloration.
  • the relative density of this sintered body was 99%.
  • Example 8 A sintered body was produced under the same conditions as in Example 1 except that each component composition was adjusted to Table 1.
  • Each component composition of the magnetic material used as the matrix of Example 8 was Co: 60 mol%, Cr: 5 mol%, and Pt: 24 mol%.
  • the oxides were Cr (BO 3 ): 4 mol%, SiO 2 : 4 mol%, and CoO: 3 mol%.
  • the ratio of Cr / B is 2.25.
  • the B / O ratio was 0.17. All satisfied the conditions of the present invention.
  • the results are also shown in Table 1.
  • the average area per particle of the oxide phase in the target was 1.1 ⁇ m 2 .
  • the appearance of the surface of the sintered body after being immersed in water had no discoloration.
  • the relative density of this sintered body was 99.2%.
  • Example 9 A sintered body was produced under the same conditions as in Example 1 except that each component composition was adjusted to Table 1.
  • Each component composition of the magnetic material used as the matrix of Example 9 was Co: 73 mol%, Cr: 2 mol%, and Pt: 17 mol%.
  • the ratio of Cr / B is 2.
  • the B / O ratio was 0.07. All satisfied the conditions of the present invention.
  • the results are also shown in Table 1.
  • the average area per one particle of the oxide phase in the target was 1.5 ⁇ m 2 .
  • the appearance of the surface of the sintered body after being immersed in water had no discoloration.
  • the relative density of this sintered body was 98%.
  • Example 10 A sintered body was produced under the same conditions as in Example 1 except that each component composition was adjusted to Table 1.
  • Each component composition of the magnetic material used as the matrix of Example 10 was Co: 65 mol%, Cr: 4 mol%, and Pt: 25 mol%.
  • the ratio of Cr / B is 1.
  • the B / O ratio was 0.27. All satisfied the conditions of the present invention.
  • the results are also shown in Table 1.
  • the average area per one particle of the oxide phase in the target was 1.6 ⁇ m 2 .
  • the appearance of the surface of the sintered body after being immersed in water had no discoloration.
  • the relative density of this sintered body was 98.8%.
  • Example 1 A sintered body was produced under the same conditions as in Example 1 except that each component composition was adjusted to Table 1.
  • Each component composition of the magnetic material used as the matrix of Comparative Example 1 was Co: 63 mol%, Cr: 5 mol%, Pt: 20 mol%, Ru: 5 mol%.
  • the oxide, B 2 O 3: 5mol% , SiO 2: was a 2 mol%.
  • the ratio of Cr / B is 0.5.
  • in the sintered body at a B / O ratio of 0.5, Cr (BO 3) Co 2 B 2 O 5, compounds of Co 3 B 2 O 6 was not confirmed. These did not satisfy the conditions of the present invention.
  • the results are also shown in Table 1.
  • the average area per particle of the oxide phase in the target was 4.3 ⁇ m 2 .
  • the appearance of the surface of the sintered body after being immersed in water was discolored.
  • the relative density of this sintered body was 96%.
  • Example 2 A sintered body was produced under the same conditions as in Example 1 except that each component composition was adjusted to Table 1. However, compound powders of Cr (BO 3 ), Co 2 B 2 O 5 , and Co 3 B 2 O 6 are not prepared in advance.
  • Each component composition of the magnetic material used as the matrix of Comparative Example 2 was Co: 68 mol%, Cr: 5 mol%, and Pt: 20 mol%.
  • the oxide, B 2 O 3: 5mol% , Cr 2 O 3: was a 2 mol%.
  • the ratio of Cr / B is 0.9.
  • the B / O ratio was 0.5.
  • the Cr / B ratio did not satisfy the conditions of the present invention.
  • the results are also shown in Table 1.
  • the average area per particle of the oxide phase in the target was 1.8 ⁇ m 2 .
  • the appearance of the surface of the sintered body after being immersed in water was discolored.
  • the relative density of this sintered body was 93%.
  • Example 3 A sintered body was produced under the same conditions as in Example 1 except that each component composition was adjusted to Table 1.
  • the composition of each component of the magnetic material serving as the matrix of Comparative Example 3 was Co: 73 mol% and Pt: 20 mol%.
  • the oxide, B 2 O 3: 6mol% , Co 3 B 2 O 6: was 1 mol%.
  • the ratio of Cr / B is zero.
  • the B / O ratio was 0.6. These did not satisfy the conditions of the present invention.
  • the results are also shown in Table 1.
  • the average area per particle of the oxide phase in the target was 5.1 ⁇ m 2 .
  • the appearance of the surface of the sintered body after being immersed in water was discolored.
  • the relative density of this sintered compact was 96.3%.
  • Example 4 A sintered body was produced under the same conditions as in Example 1 except that each component composition was adjusted to Table 1.
  • Each component composition of the magnetic material used as the matrix of Comparative Example 4 was Co: 66 mol%, Cr: 9 mol%, and B: 10 mol%. Meanwhile, oxides, CoO: 7mol%, TiO 2 : was a 8 mol%.
  • the ratio of Cr / B is 0.9.
  • the B / O ratio was 0.43.
  • the conditions of the present invention were not satisfied. Further, in the XRD measurement of the sample after sintering, generation of Cr (BO 3) was not confirmed.
  • the results are also shown in Table 1.
  • the average area per one particle of the oxide phase in the target was 3.8 ⁇ m 2 .
  • the appearance of the surface of the sintered body after being immersed in water was discolored. This was thought to be because the ratio of Cr / B was small and the amount of B was large relative to the amount of Cr, so that a large amount of boron oxide was generated and the oxide particles were coarsened.
  • the relative density of this sintered body was 99.0%.
  • Example 5 A sintered body was produced under the same conditions as in Example 1 except that each component composition was adjusted to Table 1.
  • Each component composition of the magnetic material used as the matrix of Comparative Example 5 was Co: 50 mol%, Cr: 30 mol%, and Ru: 10 mol%.
  • the oxide, B 2 O 3: 7mol% , SiO 2: was a 3 mol%.
  • the ratio of Cr / B is 2.1.
  • the B / O ratio was 0.52.
  • the conditions of the present invention were not satisfied. Further, in the XRD measurement of the sample after sintering, generation of Cr (BO 3) was not confirmed.
  • the results are also shown in Table 1.
  • the average area per one particle of the oxide phase in the target was 8.2 ⁇ m 2 .
  • the appearance of the surface of the sintered body after being immersed in water was discolored. This is considered due to the coarsening of the oxide particles due to the presence of boron oxide.
  • the relative density of this sintered body was 99.2%.
  • At least one of Cr (BO 3 ), Co 2 B 2 O 5 , and Co 3 B 2 O 6 is included in the phase of the oxide in the sintered body of the present invention, particularly the sputtering target for a magnetic recording film. This is what exists.
  • boric acid is generated by reacting with moisture and deposited on the target surface and the like. Although it was a cause of stains and dirt, this problem could be solved as well. Since particle generation can be suppressed, the magnetic recording film defect rate is reduced and the cost is reduced. This greatly contributes to the improvement of magnetic thin film quality and production efficiency. It is useful as a ferromagnetic sputtering target used for forming a magnetic thin film of a recording medium, particularly a hard disk drive recording layer.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Vapour Deposition (AREA)
  • Manufacturing Of Magnetic Record Carriers (AREA)
  • Powder Metallurgy (AREA)
  • Magnetic Record Carriers (AREA)
  • Hard Magnetic Materials (AREA)
  • Thin Magnetic Films (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

La présente invention concerne un corps fritté qui contient au moins du cobalt sous la forme d'un métal et est composé de bore et/ou d'au moins un métal choisi parmi les éléments du groupe du platine ou un alliage du métal et un oxyde, ledit corps fritté étant caractérisé en ce qu'au moins un composé choisi parmi Cr(BO3), Co2B2O5 et Co3B2O6 est contenu dans une phase composée de l'oxyde. Un corps fritté dans lequel un composé choisi parmi Cr(BO3), Co2B2O5 et Co3B2O6 est présent dans une cible peut maintenir une structure fine, et permet la production d'un corps fritté pour utilisation dans la formation de film d'enregistrement magnétique qui comprend un corps fritté qui est stable dans l'eau.
PCT/JP2014/061357 2013-04-30 2014-04-23 Corps fritté, et cible de pulvérisation pour utilisation dans la formation de film d'enregistrement magnétique qui comprend ledit corps fritté WO2014178310A1 (fr)

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SG11201506155PA SG11201506155PA (en) 2013-04-30 2014-04-23 Sintered body, and sputtering target for forming magnetic recording film produced from said sintered body
JP2014541456A JP5878242B2 (ja) 2013-04-30 2014-04-23 焼結体、同焼結体からなる磁気記録膜形成用スパッタリングターゲット
CN201480011201.XA CN105026589B (zh) 2013-04-30 2014-04-23 烧结体、包含该烧结体的磁记录膜形成用溅射靶

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WO2016133047A1 (fr) * 2015-02-19 2016-08-25 Ｊｘ金属株式会社 Cible de pulvérisation cathodique pour la formation de film mince magnétique
JP2016160530A (ja) * 2015-03-05 2016-09-05 光洋應用材料科技股▲分▼有限公司 磁気合金スパッタリングターゲット及び磁気記録媒体用記録層
WO2017090481A1 (fr) * 2015-11-27 2017-06-01 田中貴金属工業株式会社 Cible de pulvérisation cathodique
WO2020066114A1 (fr) * 2018-09-25 2020-04-02 Ｊｘ金属株式会社 Cible de pulvérisation et poudre pour produire une cible de pulvérisation
JP2020164973A (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の梱包物の作製方法及び輸送方法
CN113692457A (zh) * 2019-03-29 2021-11-23 Ｊｘ金属株式会社 溅射靶以及溅射靶的制造方法

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CN108026631A (zh) * 2015-02-19 2018-05-11 捷客斯金属株式会社 磁性体薄膜形成用溅射靶
CN108026631B (zh) * 2015-02-19 2020-02-28 捷客斯金属株式会社 磁性体薄膜形成用溅射靶
WO2016133047A1 (fr) * 2015-02-19 2016-08-25 Ｊｘ金属株式会社 Cible de pulvérisation cathodique pour la formation de film mince magnétique
JPWO2016133047A1 (ja) * 2015-02-19 2017-11-09 Ｊｘ金属株式会社 磁性体薄膜形成用スパッタリングターゲット
JP2016160530A (ja) * 2015-03-05 2016-09-05 光洋應用材料科技股▲分▼有限公司 磁気合金スパッタリングターゲット及び磁気記録媒体用記録層
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WO2017090481A1 (fr) * 2015-11-27 2017-06-01 田中貴金属工業株式会社 Cible de pulvérisation cathodique
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WO2020066114A1 (fr) * 2018-09-25 2020-04-02 Ｊｘ金属株式会社 Cible de pulvérisation et poudre pour produire une cible de pulvérisation
JPWO2020066114A1 (ja) * 2018-09-25 2021-10-21 Ｊｘ金属株式会社 スパッタリングターゲット及びスパッタリングターゲットの製造方法
JP7072664B2 (ja) 2018-09-25 2022-05-20 Ｊｘ金属株式会社 スパッタリングターゲット及びスパッタリングターゲットの製造方法
JP2020164973A (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の梱包物の作製方法及び輸送方法
WO2020202603A1 (fr) * 2019-03-29 2020-10-08 Ｊｘ金属株式会社 Procédés de fabrication et de transport d'un emballage d'une cible de pulvérisation
CN113692457A (zh) * 2019-03-29 2021-11-23 Ｊｘ金属株式会社 溅射靶以及溅射靶的制造方法

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