CN109844167A - Magnetic material sputtering target and its manufacturing method - Google Patents
Magnetic material sputtering target and its manufacturing method Download PDFInfo
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- CN109844167A CN109844167A CN201780063272.8A CN201780063272A CN109844167A CN 109844167 A CN109844167 A CN 109844167A CN 201780063272 A CN201780063272 A CN 201780063272A CN 109844167 A CN109844167 A CN 109844167A
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- 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
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- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
- G11B5/851—Coating a support with a magnetic layer by sputtering
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Abstract
A kind of magnetic material sputtering target is 500 DEG C of oxides below containing fusing point, which is characterized in that in the sputter face of the sputtering target, the mean number density for the oxide that partial size is 10 μm or more is 5/mm2Below.The issue of the present invention is to provide a kind of sputtering target and its manufacturing method, the sputtering target can efficiently reduce the generation of paradoxical discharge, powder as caused by the oxide of oxide, particularly coarse growth in sputtering target.
Description
Technical field
Remember the present invention relates to the magnetic film of the recording layer for being adapted for use in magnetic recording media etc., for example, by using perpendicular magnetic
The magnetic material sputtering target of the film forming of the membrana granulosa of the magnetic recording media of the hard disk of record mode is sputtered more particularly to being able to suppress
When paradoxical discharge, prevent powder generate magnetic material sputtering target and its manufacturing method.
Background technique
In the magnetic recording medias such as hard disk, the material for making magnetic material filming on the substrates such as glass and being formed is used
As magnetic recording layer, from the aspect of productivity height, the film forming of the magnetic recording layer is widely used using direct current (DC) power supply
Magnetron sputtering method.Magnetron sputtering method is following method: by magnet configuration in the back side of target, and make flux leakage to target surface, by
This makes magnetic flux using the charged particle in Lorentz force confined discharge plasma, so as to make highdensity plasma collection
In near target surface, therefore can be realized the high speed of film forming speed.
It is thin as the magnetism for forming the magnetic recording layer for being responsible for record in the magnetic recording field using hard disk drive as representative
The material of film is used using Co, Fe or Ni as ferromagnetism metal as the material of matrix.For example, using the magnetic of magnetic substance
Change direction be set as in the face in the direction parallel with recording surface in the recording layer of the hard disk of return to zero, use all the time with
Co makees Co-Cr base as main component, Co-Cr-Pt base strong magnetic alloy.
On the other hand, make unit record face and the direction of magnetization of magnetic substance is set as the direction vertical with recording surface
The perpendicular magnetic recording of long-pending magnetic recording amount densification is practical, it is increasingly becoming mainstream in recent years.It hangs down using this
In the magnetic recording layer of the hard disk of straight return to zero, commonly using comprising making Co-Cr-Pt base ferromagnetism as main component with Co
The composite material of alloy and non-magnetic inorganic object.Moreover, from the aspect of productivity height, frequently by using with above-mentioned material
The thin magnetic film of the magnetic recording medias such as hard disk is sputtered and made as the magnetic material sputtering target of ingredient.
As the production method of such magnetic material sputtering target, smelting process, powder metallurgic method are considered.Which kind of method passed through
It makes sputtering target and depends on required sputtering characteristic, film performance, therefore cannot treat different things as the same.However, for above-mentioned close
The sputtering target for becoming the recording layer of the hard disk of the perpendicular magnetic recording of mainstream over year is usually made by powder metallurgic method.It is former
Because being, for the sputtering target of the recording layer formation of perpendicular magnetic recording, need to divide inorganic particles equably
It is dispersed in alloy substrate, it is difficult to which such structure is realized by smelting process.
So far, the manufacture about the magnetic material sputtering target carried out by powder metallurgic method has been attempted from several sights
Point considers the method for its improvement.For example, disclose makes oxide particle point by powder metallurgic method in patent document 1,2
Sinter sputtering target obtained from being dispersed in alloy substrate, and describe by making the alloy of specific element composition with coarse
The form of the particle of change is present in alloy substrate, can reduce the magnetic conductivity of entire target, to increase by magnetic substance target
Sputter face magnetic flux (Path Through Flux；PTF), and increase the plasma density near sputter face, thus
Realize the raising of film forming speed.
In addition, disclose in patent document 3,4 makes to aoxidize by powder metallurgic method as the method considered from other viewpoints
Object particle is dispersed in alloy substrate and sinter sputtering target obtained from being sintered, and discloses and be scattered in by control
Shape, the dispersing morphology of oxide in target and obtain the technology of fine and uniform institutional framework.In these targets, as point
The oxide of granular media is insulator, therefore the reason of be likely to become paradoxical discharge according to its shape, the form of dispersion, therefore is passed through
Keep the institutional framework of target fine and homogenizes and inhibit paradoxical discharge to prevent the generation of powder.
However, these in the prior art, there are also further improve for the existing forms of the oxide in target, dispersing morphology
Leeway, it is desired to be able to more effectively inhibit paradoxical discharge and the sputtering target of the generation of powder can be prevented.In particular, vertical
After recording mode becomes mainstream, as packing density improves, the floating of the magnetic head in the magnetic recording systems such as hard disk drive is high
Degree reduces year by year, therefore the requirement to the size and number of the powder allowed on magnetic recording media just becomes to be increasingly stringenter.
Existing technical literature
Patent document
Patent document 1: Japanese Patent No. 5375707
Patent document 2: International Publication No. 2014/125897
Patent document 3: International Publication No. 2013/125469
Patent document 4: Japanese Patent No. 4975647
Summary of the invention
Problem to be solved by the invention
The issue of the present invention is to provide one kind can efficiently reduce by sputtering target oxide, particularly coarse life
The magnetic material sputtering target for being dispersed with non-magnetic material particle and its system that paradoxical discharge caused by long oxide, powder generate
Make method.
The means used to solve the problem
To solve the above-mentioned problems, present inventor has performed further investigations, as a result, it has been found that: it is low containing fusing point in sputtering target
Oxide in the case where, generate in sintering process the oxide occur melting, aggregation or reacted with other oxides, thus
The problem of being grown to partial size excessive aggregation, and by being heat-treated in advance to oxide before sintering, it can inhibit
The generation of such aggregation, it is possible thereby to reduce the yield of the powder as caused by oxide in sputtering.
Based on the discovery that the application provides invention below.
1) a kind of magnetic material sputtering target is 500 DEG C of oxides below containing fusing point, which is characterized in that splash at this
In the sputter face shot at the target, the mean number density for the oxide that partial size is 10 μm or more is 5/mm2Below.
2) it is above-mentioned 1) as described in magnetic material sputtering target, which is characterized in that the magnetic material sputtering target contain with select
Oxide from one or more of Cr, Ta, Ti, Si, Zr, Al, Nb, Co as constituent.
3) it is above-mentioned 1) or 2) as described in magnetic material sputtering target, which is characterized in that oxide in sputtering target always contains
Amount is 5 volume % or more and 50 volume % or less.
4) it is above-mentioned 1)~3) any one of as described in magnetic material sputtering target, which is characterized in that in sputtering target, Co is
55 moles of % or more and 95 mole of % are hereinafter, Cr is 40 moles of % hereinafter, Pt is 45 moles of % or less.
5) it is above-mentioned 4) as described in magnetic material sputtering target, which is characterized in that the magnetic material sputtering target contains 10 and rubs
Your % is below selected from one or more of B, N, Ti, V, Mn, Zr, Nb, Ru, Mo, Ta, W, Si, Al.
6) a kind of manufacturing method of magnetic material sputtering target, for it is above-mentioned 1)~5) any one of described in magnetic material splash
The manufacturing method shot at the target, which is characterized in that by comprising fusing point be 500 DEG C of oxides below oxide powder target sintering
It is heat-treated at a temperature of more than temperature, using the powder after being heat-treated as raw materials for sintering.
7) a kind of manufacturing method of magnetic material sputtering target, for it is above-mentioned 1)~5) any one of described in magnetic material splash
The manufacturing method shot at the target, which is characterized in that by the oxide powder other than fusing point is 500 DEG C of oxides below in target
It is heat-treated at a temperature of more than sintering temperature, using the powder after being heat-treated as raw materials for sintering.
8) it is above-mentioned 6) or 7) as described in magnetic material sputtering target manufacturing method, wherein the manufacturing method is included in
In the process of 800 DEG C or more and 1900 DEG C heat treated below in atmosphere.
9) it is above-mentioned 6) as described in magnetic material sputtering target manufacturing method, wherein the manufacturing method include will carry out
The particle size adjustment of oxide powder after heat treatment to average grain diameter is 5 μm of processes below.
10) it is above-mentioned 6)~9) any one of as described in magnetic material sputtering target manufacturing method, wherein the manufacturer
Method includes the process for keeping carrying out hot pressed sintering at 500 DEG C~1400 DEG C of temperature.
Invention effect
The magnetic material sputtering target for being dispersed with non-magnetic material particle of the invention facilitate sputtering when by coarse oxygen
The reduction that the inhibition of paradoxical discharge caused by compound, powder generate can greatly improve characteristic compared with previous sputtering target.
Following excellent results are played as a result: can obtain improving bring cost improvement effect by further yield rate.
Detailed description of the invention
Fig. 1 is the schematic diagram being illustrated for the partial size to oxide particle of the invention.
Fig. 2 is the figure for indicating the structure observation position of sputtering target of the invention.
Fig. 3 is the structure observation image of the sputtering target (sputtering surface side) of embodiment 1 obtained using laser microscope.
Fig. 4 is the structure observation image of the sputtering target (sputtering surface side) of comparative example 1 obtained using laser microscope.
Fig. 5 is the EPMA element distribution image of the oxide in the sputtering target of comparative example 1.
Specific embodiment
Fusing point is being used to be 500 DEG C of oxides (hereinafter, sometimes referred to as low melting point oxide) below as non magnetic material
In the case where the raw material of material, such low melting point oxide is melted in sintering sometimes, with its own or other oxides
It reacts and forms aggregation.When there is aggregation, coarsening oxide in sintered body (sputtering target), sometimes in sputtering as
Starting point is abnormal electric discharge or the disengaging of coarsening oxide etc. and generates powder, and becoming reduces film quality and then make to produce
The reason of yield rate of product reduces.
It is a feature of the present invention that by being heat-treated in advance to oxide, oxide when inhibiting by being sintered it is molten
The formation of aggregation caused by melting, reduce the coarse oxide in sputtering target there are ratios.That is, magnetic material of the invention
Sputtering target is characterized in that, contain fusing point be 500 DEG C of oxides below as non-magnetic material particle in the case where, will splash
The mean number Auto-regulating System of Density of Heavy Medium for the oxide that partial size present in shooting at the target is 10 μm or more is 5/mm2Below.
The shape (floor map) for the oxide that will be present in sputtering target is shown in Fig. 1.As shown in Figure 1, oxide
Flat shape is not necessarily positive round or elliptical shape, therefore, in the present invention, will draw most in the flat shape of oxide
The diameter of big inscribed circle is defined as partial size.In addition, illustrating that the schematic diagram of the structure observation position of sputtering target in Fig. 2.Such as Fig. 2
Shown, the center to target and total 10 positions at the 1/2 of radius (r) carry out structure observation, by the oxygen in each observation tissue
The average value of compound number density is as mean number density.At this point, in order to accurately hold the shape of oxide, in 175 μ ms
It is observed in 1433 μm of the visual field.
In the case where the use of fusing point being 500 DEG C of oxides below, the significant clustering phenomena generated when being sintered.As molten
Point is 500 DEG C of oxides below, can enumerate such as diboron trioxide (B2O3)。B2O3It is as magnetic material sputtering target
The material that non-magnetic material is commonly used, therefore, although being referred to B in the application2O3As long as but fusing point is 500 DEG C or less
Oxide, same phenomenon will be generated, thus in raw materials for sintering using remove B2O3The feelings of low-melting oxide in addition
It, also can be using the present invention under condition.
In raw materials for sintering containing fusing point be 500 DEG C of oxide (low melting point oxides) below in the case where, be sintered
Shi Fasheng melting, to be remained in the form of coarse oxide aggregate in sintered body.As the such aggregation of inhibition
Generation means, have following methods: 1) being heat-treated low melting point oxide and other oxides together, to synthesize
The method of compound (composite oxides) with different melting points；2) by advance to the oxide other than low melting point oxide into
Row heat treatment, to be not susceptible to the method reacted and (make reactive reduction) with low melting point oxide in sintering.
As the oxide other than low melting point oxide, can enumerate with selected from Cr, Ta, Ti, Si, Zr, Al, Nb,
Oxide of one or more of the Co as constituent.These oxides are with the oxide of single element or theirs is compound
Oxide and it is present in sputtering target with the form of the composite oxides of above-mentioned low melting point oxide.In sputtering target, include
The total content of oxide including low melting point oxide is preferably set to 5 volume % or more and 50 volume % or less.By by oxygen
The total volume ratio set of compound is 5 volume % or more, available good magnetic characteristic.In addition, by by the total of oxide
Volume ratio is set as 50 volume % hereinafter, dispersing with can making oxide fine uniform structure.Further preferably 20 volume % with
Upper and 40 volume % or less.
For magnetic material sputtering target of the invention, in sputtering target, contain 55 moles of % or more and 95 mole of %
Co below can rub as optional member containing 45 moles of % Pt below, 40 moles of % Cr below, Pt and Cr for 0
You are %.It forms the mainly magnetic characteristic required by magnetic recording layer and determines.In order to tighter control magnetic characteristic, preferably by Co's
Content is set as 60 moles of % or more and 85 mole of % hereinafter, the content of Pt is set as 25 moles of % hereinafter, by the content of Cr
It is set as 20 moles of % or less.In addition, in order to improve magnetic characteristic, containing 10 moles of % it is below selected from B, N, Ti, V, Mn, Zr,
One or more of Nb, Ru, Mo, Ta, W, Si, Al are effective.
Magnetic material sputtering target of the invention can be used powder sintering, for example make by the following method.
Firstly, preparing Co powder, Pt powder, Cr powder as powder such as magnetic material and B, Ti, V as additive.
For these powder, the powder of single element not only can be used, alloyed powder also can be used.It is preferable to use partial sizes at 1 μm
Powder in the range of~10 μm.When partial size is 1 μm~10 μm, mixing more evenly may be implemented, segregation and thick can be prevented
Big crystallization.In the case where the partial size of metal powder is greater than 10 μm, non-magnetic material will not be uniformly dispersed sometimes, in addition,
In the case that the partial size of metal powder is less than 1 μm, compositional deviation institute's phase of the influence by the oxidation of metal powder and target is generated sometimes
The problem of composition of prestige.It should be noted that it should be understood that the particle size range only preferred range, exceeds the model
Enclosing is not negative condition of the invention.
Prepare be comprising fusing point it is including 500 DEG C of oxides below, using Cr, Ta, Ti, Si etc. as the oxygen of constituent
The powder of compound is as non-magnetic material.It is expected that the powder using the partial size of oxide in the range of 1 μm~5 μm.With metal
The partial size of powder is equal or when below it, is easy to be crushed, when being mixed with above-mentioned metal powder, non-magnetic material powder
It is not easy to assemble each other, its can be made evenly dispersed.It should be noted that it should be understood that the particle size range is only preferred
Range, be not negative condition of the invention beyond the range.
Then, the prior heat treatment of the oxide as emphasis of the invention is illustrated.As previously mentioned, fusing point is
500 DEG C of oxides below are melted in the sintering of target, to be easy to generate aggregation, therefore, feature of the invention exists
In, by being heat-treated at a temperature of the sintering temperature than target is high to oxide in advance, 1) low melting point oxide is synthesized
For the higher composite oxides of fusing point or 2) reactivity of the oxide other than low melting point oxide is reduced.
As it is above-mentioned 1), by being 500 DEG C of oxides (low melting point oxide) below and other oxides by fusing point
The mixed-powder of (that is, fusing point is higher than 500 DEG C oxide) more than the sintering temperature of target at a temperature of be heat-treated, make low
Refractory oxides and other oxides are synthesized and form the higher composite oxides of fusing point, it is possible thereby to inhibit the burning in target
With the aggregation of oxide fusion when knot.
As it is above-mentioned 2), by only to its other than fusing point is 500 DEG C of oxides (low melting point oxide) below
Its oxide (fusing point is higher than 500 DEG C of oxide) more than the sintering temperature of target at a temperature of be heat-treated, inhibit in target
Sintering when reacted with low melting point oxide, inhibit the coarsening of oxide.
The heat treatment of oxide powder carries out more than the sintering temperature of target, preferably in an atmosphere 800 DEG C or more and
1900 DEG C or less.When lower than 800 DEG C, the heat treatment of oxide powder is not sufficiently effective sometimes, on the other hand, is higher than 1900 DEG C
When, energy cost is got higher, therefore not preferably.The heat treatment time of oxide powder preferably carries out 2 hours or more.Oxide powder
Heat treatment after, it is preferable to use mortar etc. crushes oxide powder, thus adjust partial size so that average grain diameter be 5 μm with
Under.If it is powder of the average grain diameter in 5 μm or less of range, then the non-magnetic material powder when being mixed with above-mentioned metal powder
End is not easy to assemble each other, it can be made to be uniformly dispersed.
Then, above-mentioned raw material powder and oxide heat treated powder are weighed with obtain it is desired form, use ball
Method well known to grinding machine etc. is mixed while crushing.Later, using pressure sintering to obtained mixed-powder in vacuum
It is formed and is sintered in atmosphere or inert gas atmosphere.Other than above-mentioned hot pressing, it can also be burnt using discharge plasma
The various pressure sintering methods such as connection.In particular, HIP sintering method is effective to the density for improving sintered body.The sintering of target
When holding temperature depend on target at being grouped as, be preferably set within the temperature range of 500 DEG C~1400 DEG C.It will obtain in this way
Sintered body using lathe process at desired shape, it is possible thereby to manufacture sputtering target of the invention.
Evaluation method of the invention including aftermentioned embodiment, comparative example etc. is as described below.
(about the structure observation of target and a number density of oxide particle)
The evaluation of the tissue on target surface is carried out using the enlarged drawing obtained using laser microscope.Carried out grinding,
In the pretreated target surfaces such as cleaning, as shown in Fig. 2, using laser microscope at the center (1 point) of target and radius 1/2 (9
A point) total 10 points carry out structure observations, and shoot respective observation image.About observation multiple, it is set as sight plane
1433 μm of 1075 μ m of product enables to the shape for accurately evaluating oxide.Then, by the group of 10 points extracted
It knits image and is converted to binary image.Threshold value when carrying out binaryzation is set in, matrix as main component is made with metal component
Between the difference of the tone on the boundary of oxide particle.In general, according to the poor contrast between matrix and oxide particle, it can
With the boundary both clearly identified, but can also be improved point by and with the processing such as techniques of discriminant analysis, histogram of difference method
From precision.It then, is 10 to partial size for carrying out the observation image of each point of the observation image of 10 points after binaryzation in this way
μm or more the quantity of oxide particle counted, calculate divided by per unit area obtained from field of view area
Number density finds out the average value (a number density) of 10 points.
(volume ratio about the oxide in target)
In the present invention, about the volume ratio of the oxide in sputtering target, to be obtained in above-mentioned using laser microscope
Observation image in be equivalent to the area ratio (area ratio [%]=by binaryzation point of oxide in entire field of view
Oxide area obtained from analysis [μm2]/field area [μm2] × 100) value evaluated.Oxidation in entire field of view
The area ratio of object is actually the ratio of area shown by oxide in a two-dimensional plane, is not the body in three-dimensional space
Long-pending ratio still, can be by the area in two-dimensional surface under the premise of particle isotropically disperses in all directions
Ratio is considered as the volume ratio in three-dimensional space.It should be noted that confirming according to the oxide of the observation picture appraisal
Volume ratio (volume %) and the volume ratio for the oxide evaluated according to the weight and density of raw material are not significantly different.
Embodiment
The present invention is concretely demonstrated based on embodiment etc..For easy understanding the record of embodiment below etc. is
The concrete example of technology contents of the invention, technical scope of the invention are not limited by these concrete examples.
(embodiment 1, comparative example 1)
Prepare 3 μm of average grain diameter of Co powder, 3 μm of average grain diameter of Pt powder, 3 μm of average grain diameter of Cr powder as gold
Belong to the raw material powder of ingredient, prepares 1 μm of average grain diameter of B2O3Powder, 1 μm of average grain diameter of TiO2Powder, 1 μm of average grain diameter
SiO2Powder, 1 μm of average grain diameter of Cr2O3The raw material powder of powder, 1 μm of average grain diameter of CoO powder as oxide components.
These powder are weighed to obtain forming for molar ratio below.Composition is as follows.
Composition: 70Co-4Cr-10Pt-4B2O3-2TiO2-2SiO2-2Cr2O3- 6CoO moles of %
Then, in embodiment 1, by the TiO as the raw material powder of oxide components2Powder, SiO2Both oxygen of powder
The mixing of compound powder, and the mixed-powder is heat-treated.Heat treatment under the air atmosphere of normal pressure, at 1050 DEG C into
Row 5 hours.Oxide powder after heat treatment is first cooled to room temperature by the way that furnace is cold, then for subsequent mixed processes.
On the other hand, it in comparative example 1, is not heat-treated.
Then, using about 7 liters of ball capacity of planetary motion type mixer that the oxide powder being heat-treated is (only real
Apply example 1), be not heat-treated raw material powder co-grinding 10 minutes of oxide powder and metal component, then by it
With the TiO as crushing medium2Ball is enclosed together in the ball mill tank of 10 liters of capacity, is made its rotation 20 hours and is mixed.
Then, obtained mixed-powder is filled into carbon molding jig, in vacuum atmosphere, 850 DEG C of temperature, 2 hours retention times,
Hot pressing is carried out under conditions of moulding pressure 30MPa, to obtain sintered body.Then, machining is carried out to it and obtained
Diameter is 165.1mm, the disk-shaped sputtering target with a thickness of 5mm.
For obtained sputtering target, institutional framework is seen using laser microscope after being ground to surface
It examines.Respective organization chart picture is shown in Fig. 3 (embodiment 1), Fig. 4 (comparative example 1).In addition, being 1075 μ about each field area
The average particle quantity in 10 visuals field of the oxide that partial size present in the organization chart picture of m × 1433 μm is 10 μm or more,
It is 2.9 in embodiment 1, mean number density is 1.88/mm2, meet the scope of the present invention.On the other hand, in comparative example 1
In be 12.5, mean number density be 8.11/mm2, have exceeded the scope of the present invention.
Here, the oxide in the sputtering target of comparative example 1 is shown and is obtained using electron beam microscopic analyzer (EPMA)
The distribution diagram of element arrived.As shown in figure 5, can be confirmed that oxide is the composite oxides comprising Co-B-O, Si-B-O.Think this
It is the B in sintering2O3Melting occurs, assembles and is formed.
Then, powder evaluation has been carried out and sputtering target to be installed on DC magnetic control sputtering device to and implemented sputtering.It splashes
The condition of penetrating is set as input power 1kW, sputtering time 20 seconds, Ar atmosphere pressures 1.7Pa.Then, it is measured using powder counter
The number for the powder that the diameter being attached on substrate is 0.07 μm or more.As a result: powder number is 51 in embodiment 1
It is a, it is 129 in 1 medium silt number of comparative example, observes significant difference.
(embodiment 2, comparative example 2)
Prepare the raw material powder of 3 μm of average grain diameter of Co powder, 3 μm of average grain diameter of Pt powder as metal component, it is quasi-
The B of standby 1 μm of average grain diameter2O3Powder, 1 μm of average grain diameter of TiO2Powder, 1 μm of average grain diameter of SiO2Powder is as oxide
The raw material powder of ingredient.These powder are weighed to obtain forming for molar ratio below.Composition is as follows.
Composition: 65Co-20Pt-5B2O3-5TiO2-5SiO2Mole %
Then, in example 2, by the TiO as the raw material powder of oxide components2Powder, SiO2Both oxygen of powder
The mixing of compound powder, and the mixed-powder is heat-treated.The condition of heat treatment is same as Example 1.After heat treatment
Oxide powder is first cooled to room temperature by the way that furnace is cold, then for subsequent mixed processes.On the other hand, in comparative example 2
In, it is not heat-treated.
Then, using about 7 liters of ball capacity of planetary motion type mixer that the oxide powder being heat-treated is (only real
Apply example 2), be not heat-treated raw material powder co-grinding 10 minutes of oxide powder and metal component, then by it
With the TiO as crushing medium2Ball is enclosed together in the ball mill tank of 10 liters of capacity, is made its rotation 20 hours and is mixed.
Then, obtained mixed-powder is filled into carbon molding jig, in vacuum atmosphere, 850 DEG C of temperature, 2 hours retention times,
Hot pressing is carried out under conditions of moulding pressure 30MPa, to obtain sintered body.Then, machining is carried out to it and obtained
Diameter is 165.1mm, the disk-shaped sputtering target with a thickness of 5mm.
For obtained sputtering target, institutional framework is observed similarly to Example 1, as a result: about
Each field area is 10 visuals field of the oxide that partial size present in the organization chart picture of 1433 μm of 1075 μ m is 10 μm or more
Number average particle, be in example 2 7.0, mean number density be 4.54/mm2, meet the scope of the present invention.Separately
It on the one hand, is 10.0 in comparative example 2, mean number density is 6.49/mm2, have exceeded the scope of the present invention.Then,
Pass through sputtering test similarly to Example 1 to the target to be evaluated, as a result: about the powder observed on a silicon substrate
The powder number that grain diameter is 0.07 μm or more, is in example 2 76, is 88 in comparative example 2, observes significance difference
It is different.
(embodiment 3, comparative example 3)
Prepare the raw material powder of 3 μm of average grain diameter of Co powder, 3 μm of average grain diameter of Cr powder as metal component, it is quasi-
The B of standby 1 μm of average grain diameter2O3Powder, 1 μm of average grain diameter of TiO2Powder, 1 μm of average grain diameter of SiO2Powder is as oxide
The raw material powder of ingredient.These powder are weighed to obtain forming for molar ratio below.Composition is as follows.
Composition: 65Co-20Cr-5B2O3-5TiO2-5SiO2Mole %
Then, in embodiment 3, by the TiO as the raw material powder of oxide components2Powder, SiO2Both oxygen of powder
The mixing of compound powder, and the mixed-powder is heat-treated.The condition of heat treatment is same as Example 1.After heat treatment
Oxide powder is first cooled to room temperature by the way that furnace is cold, then for subsequent mixed processes.On the other hand, in comparative example 3
In, it is not heat-treated.
Then, using about 7 liters of ball capacity of planetary motion type mixer that the oxide powder being heat-treated is (only real
Apply example 3), be not heat-treated raw material powder co-grinding 10 minutes of oxide powder and metal component, then by it
With the TiO as crushing medium2Ball is enclosed together in the ball mill tank of 10 liters of capacity, is made its rotation 20 hours and is mixed.
Then, obtained mixed-powder is filled into carbon molding jig, in vacuum atmosphere, 850 DEG C of temperature, 2 hours retention times,
Hot pressing is carried out under conditions of moulding pressure 30MPa, to obtain sintered body.Then, machining is carried out to it and obtained
Diameter is 165.1mm, the disk-shaped sputtering target with a thickness of 5mm.
For obtained sputtering target, institutional framework is observed similarly to Example 1, as a result: about
Each field area is 10 visuals field of the oxide that partial size present in the organization chart picture of 1433 μm of 1075 μ m is 10 μm or more
Number average particle, be in embodiment 3 3.5, mean number density be 2.27/mm2, meet the scope of the present invention.Separately
It on the one hand, is 11.2 in comparative example 3, mean number density is 7.27/mm2, have exceeded the scope of the present invention.Then,
Pass through sputtering test similarly to Example 1 to the target to be evaluated, as a result: about the powder observed on a silicon substrate
The powder number that grain diameter is 0.07 μm or more, is in embodiment 3 70, is 118 in comparative example 3, observes significance difference
It is different.
(embodiment 4, comparative example 4)
Prepare the raw material powder of 3 μm of average grain diameter of Co powder, 3 μm of average grain diameter of Cr powder as metal component, it is quasi-
The B of standby 1 μm of average grain diameter2O3Powder, 1 μm of average grain diameter of TiO2Raw material powder of the powder as oxide components.Weigh these
Powder is to obtain forming for molar ratio below.Composition is as follows.
Composition: 65Co-20Cr-5B2O3-10TiO2Mole %
Then, by the B as the raw material powder of oxide components2O3Powder, TiO2Both oxide powders of powder are mixed
It closes, and the mixed-powder is heat-treated.Heat treatment carries out 5 hours under the air atmosphere of normal pressure, at 950 DEG C.Heat
Treated, and oxide powder is first cooled to room temperature by the way that furnace is cold, then for subsequent mixed processes.On the other hand, exist
In comparative example 4, it is not heat-treated.
Then, using about 7 liters of ball capacity of planetary motion type mixer that the oxide powder being heat-treated is (only real
Apply example 4), be not heat-treated raw material powder co-grinding 10 minutes of oxide powder and metal component, then by it
With the TiO as crushing medium2Ball is sealed together into 10 liters of capacity of ball mill tank, is made its rotation 20 hours and is mixed
It closes.Then, obtained mixed-powder is filled into carbon molding jig, in vacuum atmosphere, 850 DEG C of temperature, retention time 2 it is small
When, carry out hot pressing under conditions of moulding pressure 30MPa, to obtain sintered body.Then, machining is carried out to it and obtained
Diameter is 165.1mm, the disk-shaped sputtering target with a thickness of 5mm.
For obtained sputtering target, institutional framework is observed similarly to Example 1, as a result: about
Each field area is 10 visuals field of the oxide that partial size present in the organization chart picture of 1433 μm of 1075 μ m is 10 μm or more
Number average particle, be in example 4 7.2, mean number density be 4.67/mm2, meet the scope of the present invention.Separately
It on the one hand, is 15.5 in comparative example 4, mean number density is 10.06/mm2, have exceeded the scope of the present invention.Then,
Pass through sputtering test similarly to Example 1 to the target to be evaluated, as a result: about the powder observed on a silicon substrate
The powder number that grain diameter is 0.07 μm or more, is in example 4 98, is 217 in comparative example 2, observes significance difference
It is different.
(embodiment 5, comparative example 5)
Prepare the raw material powder of 3 μm of average grain diameter of Co powder, 3 μm of average grain diameter of Cr powder as metal component, it is quasi-
The B of standby 1 μm of average grain diameter2O3Powder, 1 μm of average grain diameter of SiO2Raw material powder of the powder as oxide components.Weigh these
Powder is to obtain forming for molar ratio below.Composition is as follows.
Composition: 65Co-20Cr-5B2O3-10SiO2Mole %
Then, in embodiment 5, by the B as the raw material powder of oxide components2O3Powder, SiO2Both oxygen of powder
The mixing of compound powder, and the mixed-powder is heat-treated.Heat treatment under the air atmosphere of normal pressure, at 850 DEG C into
Row 5 hours.Oxide powder after heat treatment is first cooled to room temperature by the way that furnace is cold, then for subsequent mixed processes.
On the other hand, it in comparative example 5, is not heat-treated.
Then, using about 7 liters of ball capacity of planetary motion type mixer that the oxide powder being heat-treated is (only real
Apply example 5), be not heat-treated raw material powder co-grinding 10 minutes of oxide powder and metal component, then by it
With the TiO as crushing medium2Ball is enclosed together in the ball mill tank of 10 liters of capacity, is made its rotation 20 hours and is mixed.
Then, obtained mixed-powder is filled into carbon molding jig, in vacuum atmosphere, 850 DEG C of temperature, 2 hours retention times,
Hot pressing is carried out under conditions of moulding pressure 30MPa, to obtain sintered body.Then, machining is carried out to it and obtained
Diameter is 165.1mm, the disk-shaped sputtering target with a thickness of 5mm.
For obtained sputtering target, institutional framework is observed similarly to Example 1, as a result: about
Each field area is 10 visuals field of the oxide that partial size present in the organization chart picture of 1433 μm of 1075 μ m is 10 μm or more
Number average particle, in embodiment 5 be 5.1, mean number density be 3.31/mm2, meet the scope of the present invention.Separately
It on the one hand, is 7.9 in comparative example 5, mean number density is 5.13/mm2, have exceeded the scope of the present invention.Then, right
The target passes through sputtering test similarly to Example 1 and is evaluated, as a result: about the powder observed on a silicon substrate
The powder number that diameter is 0.07 μm or more is 66 in embodiment 5, is 77 in comparative example 5, observes significant difference.
(embodiment 6, comparative example 6)
Prepare the raw material powder of 3 μm of average grain diameter of Co powder, 3 μm of average grain diameter of Cr powder as metal component, it is quasi-
The B of standby 1 μm of average grain diameter2O3Powder, 1 μm of average grain diameter of Cr2O3Raw material powder of the powder as oxide components.Weigh this
A little powder are to obtain forming for molar ratio below.Composition is as follows.
Composition: 65Co-20Cr-5B2O3-10Cr2O3Mole %
Then, in embodiment 6, by the B as the raw material powder of oxide components2O3Powder, Cr2O3Powder both
Oxide powder mixing, and the mixed-powder is heat-treated.It is heat-treated under the air atmosphere of normal pressure, at 850 DEG C
It carries out 5 hours.Oxide powder after heat treatment is first cooled to room temperature by the way that furnace is cold, then for subsequent mixing work
Sequence.On the other hand, it in comparative example 6, is not heat-treated.
Then, using about 7 liters of ball capacity of planetary motion type mixer that the oxide powder being heat-treated is (only real
Apply example 6), be not heat-treated raw material powder co-grinding 10 minutes of oxide powder and metal component, then by it
With the TiO as crushing medium2Ball is enclosed together in the ball mill tank of 10 liters of capacity, is made its rotation 20 hours and is mixed.
Then, obtained mixed-powder is filled into carbon molding jig, in vacuum atmosphere, 850 DEG C of temperature, 2 hours retention times,
Hot pressing is carried out under conditions of moulding pressure 30MPa, to obtain sintered body.Then, machining is carried out to it and obtained
Diameter is 165.1mm, the disk-shaped sputtering target with a thickness of 5mm.
For obtained sputtering target, institutional framework is observed similarly to Example 1, as a result: about
Each field area is 10 visuals field of the oxide that partial size present in the organization chart picture of 1433 μm of 1075 μ m is 10 μm or more
Number average particle, in embodiment 6 be 7.1, mean number density be 4.61/mm2, meet the scope of the present invention.Separately
It on the one hand, is 14.3 in comparative example 6, mean number density is 9.28/mm2, have exceeded the scope of the present invention.Then,
Pass through sputtering test similarly to Example 1 to the target to be evaluated, as a result: about the powder observed on a silicon substrate
The powder number that grain diameter is 0.07 μm or more is 102 in embodiment 6, is 182 in comparative example 6, observes significance difference
It is different.
(embodiment 7, comparative example 7)
Prepare the raw material powder of 3 μm of average grain diameter of Co powder, 3 μm of average grain diameter of Cr powder as metal component, it is quasi-
The B of standby 1 μm of average grain diameter2O3Powder, 1 μm of average grain diameter of Ta2O5Raw material powder of the powder as oxide components.Weigh this
A little powder are to obtain forming for molar ratio below.Composition is as follows.
Composition: 65Co-20Cr-5B2O3-10Ta2O5Mole %
Then, in embodiment 7, by the B as the raw material powder of oxide components2O3Powder, Ta2O5Powder both
Oxide powder mixing, and the mixed-powder is heat-treated.It is heat-treated under the air atmosphere of normal pressure, at 1050 DEG C
It carries out 5 hours.Oxide powder after heat treatment is first cooled to room temperature by the way that furnace is cold, then for subsequent mixing work
Sequence.On the other hand, it in comparative example 7, is not heat-treated.
Then, using about 7 liters of ball capacity of planetary motion type mixer that the oxide powder being heat-treated is (only real
Apply example 7), be not heat-treated raw material powder co-grinding 10 minutes of oxide powder and metal component, then by it
With the TiO as crushing medium2Ball is enclosed together in the ball mill tank of 10 liters of capacity, is made its rotation 20 hours and is mixed.
Then, obtained mixed-powder is filled into carbon molding jig, in vacuum atmosphere, 850 DEG C of temperature, 2 hours retention times,
Hot pressing is carried out under conditions of moulding pressure 30MPa, to obtain sintered body.Then, machining is carried out to it and obtained
Diameter is 165.1mm, the disk-shaped sputtering target with a thickness of 5mm.
For obtained sputtering target, institutional framework is observed similarly to Example 1, as a result: about
Each field area is 10 visuals field of the oxide that partial size present in the organization chart picture of 1433 μm of 1075 μ m is 10 μm or more
Number average particle, in embodiment 7 be 74.3, mean number density be 2.79/mm2, meet the scope of the present invention.Separately
It on the one hand, is 11.5 in comparative example 7, mean number density is 7.47/mm2, have exceeded the scope of the present invention.Then,
Pass through sputtering test similarly to Example 1 to the target to be evaluated, as a result: about the powder observed on a silicon substrate
The powder number that grain diameter is 0.07 μm or more is 84 in embodiment 7, is 161 in comparative example 7, observes significance difference
It is different.
It the above results are shown in table 1.
Industrial applicability
The present invention is able to suppress in the institutional framework of magnetic material sputtering target especially as caused by low melting point oxide
Aggregation, so as to inhibit the generation of the paradoxical discharge as caused by coarse oxide, reduction powder in sputtering.Thus it obtains
Following excellent results: can further expansion by yield rate improve bring cost improvement effect.The present invention is used as to be remembered for magnetic
The magnetic material sputtering target of the film forming of the thin magnetic film, particularly hard disk drive recording layer of recording medium is useful.
Claims (10)
1. a kind of magnetic material sputtering target is 500 DEG C of oxides below containing fusing point, which is characterized in that in the sputtering target
Sputter face in, the mean number density for the oxide that partial size is 10 μm or more is 5/mm2Below.
2. magnetic material sputtering target as described in claim 1, which is characterized in that the magnetic material sputtering target contains to be selected from
The oxide of one or more of Cr, Ta, Ti, Si, Zr, Al, Nb, Co as constituent.
3. magnetic material sputtering target as claimed in claim 1 or 2, which is characterized in that the total content of the oxide in sputtering target
For 5 volume of volume %~50 %.
4. magnetic material sputtering target according to any one of claims 1 to 3, which is characterized in that in sputtering target, Co 55
Mole % or more and 95 mole of % is hereinafter, Cr is 40 moles of % hereinafter, Pt is 45 moles of % or less.
5. magnetic material sputtering target as claimed in claim 4, which is characterized in that the magnetic material sputtering target contains 10 and rubs
Your % is below selected from one or more of B, N, Ti, V, Mn, Zr, Nb, Ru, Mo, Ta, W, Si, Al.
6. a kind of manufacturing method of magnetic material sputtering target sputters for magnetic material according to any one of claims 1 to 5
The manufacturing method of target, which is characterized in that by comprising fusing point be 500 DEG C of oxides below oxide powder target sintering temperature
Du or more at a temperature of be heat-treated, using the powder after being heat-treated as raw materials for sintering.
7. a kind of manufacturing method of magnetic material sputtering target sputters for magnetic material according to any one of claims 1 to 5
The manufacturing method of target, which is characterized in that by the oxide powder other than fusing point is 500 DEG C of oxides below target burning
It is heat-treated at a temperature of more than junction temperature, using the powder after being heat-treated as raw materials for sintering.
8. the manufacturing method of magnetic material sputtering target as claimed in claims 6 or 7, wherein the manufacturing method is included in big
In the process of 800 DEG C or more and 1900 DEG C heat treated below in gas.
9. the manufacturing method of magnetic material sputtering target as claimed in claim 6, wherein the manufacturing method includes that will carry out heat
The particle size adjustment of treated oxide powder to average grain diameter is 5 μm of processes below.
10. the manufacturing method of the magnetic material sputtering target as described in any one of claim 6~9, wherein the manufacturing method
It include the process for keeping carrying out hot pressed sintering at 500 DEG C~1400 DEG C of temperature.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
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| JP2016255597 | 2016-12-28 | ||
| JP2016-255597 | 2016-12-28 | ||
| PCT/JP2017/043990 WO2018123500A1 (en) | 2016-12-28 | 2017-12-07 | Magnetic material sputtering target and method for manufacturing same |
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| CN109844167B CN109844167B (en) | 2022-01-04 |
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| JP (1) | JP6734399B2 (en) |
| CN (1) | CN109844167B (en) |
| MY (1) | MY191374A (en) |
| SG (1) | SG11201903240PA (en) |
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| WO (1) | WO2018123500A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114600190A (en) * | 2019-11-01 | 2022-06-07 | 田中贵金属工业株式会社 | Sputtering target for heat-assisted magnetic recording medium |
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| CN112739846A (en) * | 2018-09-25 | 2021-04-30 | Ｊｘ金属株式会社 | Sputtering target and powder for producing sputtering target |
| WO2021010490A1 (en) * | 2019-07-18 | 2021-01-21 | 田中貴金属工業株式会社 | Sputtering target for magnetic recording medium |
| TWI834072B (en) * | 2021-10-22 | 2024-03-01 | 光洋應用材料科技股份有限公司 | Ru-al alloy target and method of preparing the same |
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| Publication number | Publication date |
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| MY191374A (en) | 2022-06-21 |
| TWI753073B (en) | 2022-01-21 |
| JPWO2018123500A1 (en) | 2019-03-28 |
| WO2018123500A1 (en) | 2018-07-05 |
| TW201835361A (en) | 2018-10-01 |
| CN109844167B (en) | 2022-01-04 |
| SG11201903240PA (en) | 2019-05-30 |
| JP6734399B2 (en) | 2020-08-05 |
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