CN105793465B - Magnetic recording film, which is formed, uses sputtering target and its manufacturing method - Google Patents
Magnetic recording film, which is formed, uses sputtering target and its manufacturing method Download PDFInfo
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- CN105793465B CN105793465B CN201480063680.XA CN201480063680A CN105793465B CN 105793465 B CN105793465 B CN 105793465B CN 201480063680 A CN201480063680 A CN 201480063680A CN 105793465 B CN105793465 B CN 105793465B
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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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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
-
- 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
-
- 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
- C22C2202/00—Physical properties
- C22C2202/02—Magnetic
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Vapour Deposition (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
一种含有C的FePt基磁记录膜形成用溅射靶，其特征在于，在与溅射面垂直的截面的抛光面中，Fe‑Pt合金相的平均厚度为10μm以上。本发明的课题在于提供抑制了溅射时由于异常放电而导致的粉粒产生的强磁性材料溅射靶。
A sputtering target for forming a FePt-based magnetic recording film containing C, characterized in that the average thickness of the Fe-Pt alloy phase is 10 μm or more in the polished surface of the cross-section perpendicular to the sputtering surface. An object of the present invention is to provide a ferromagnetic material sputtering target that suppresses the generation of particles due to abnormal discharge during sputtering.
Description
Technical field
The present invention relates to the magnetic recording layers in the magnetic film of magnetic recording media, especially hamr medium
Ferromagnetic material sputtering target used in film forming；It is related to that stable put can be obtained when being sputtered using magnetic control sputtering device
Electric and powder generates few FePt base ferromagnetic material sputtering target.
Background technique
In with the field for the magnetic recording media that HDD (hard disk drive) is representative, as the thin magnetic film for undertaking record
Material, use using Co, Fe or Ni as ferromagnetism metal as the material of matrix.For example, using return to zero in face
The recording layer of hard disk uses always with Co Co-Cr base as main component or Co-Cr-Pt base strong magnetic alloy.In addition, using close
The recording layer of the hard disk of the perpendicular magnetic recording of Nian Laiyi functionization is used comprising with Co Co-Cr-Pt as main component more
The composite material of base strong magnetic alloy and non-magnetic inorganic composition granule.Also, from the viewpoint of productivity height, hard disk equimagnetic note
The thin magnetic film of recording medium is sputtered by using by the ferromagnetic material sputtering target of ingredient of above-mentioned material in most cases
And it makes.
On the other hand, the packing density of magnetic recording media rapidly increases year by year, it is believed that in the future from 100 current gigabit ratios
The surface density of special (Gbit)/square inch reaches 1,000,000,000,000 bits (Tbit)/square inch.Packing density reach 1,000,000,000,000 bits/
When square inch, the size of record bit (bit) is less than 10nm, in such a case, it is possible to expect as caused by thermal fluctuation
Superparamagnetic becomes problem, and is anticipated that the magnetic recording media used till now, for example by adding in Co-Cr based alloy
Add Pt and improves the material of crystal magnetic anisotropy or further add B thereto and reduce the magnetic coupling between magnetic-particle
The medium of conjunction is insufficient.This is because showing ferromagnetic particle needs with 10nm dimensionally stable below has
Higher crystal magnetic anisotropy.
For the above reasons, there is L10The FePt phase of structure attracts attention as super high-density recording medium material.
In addition, having L10The FePt phase of structure is excellent in terms of corrosion resistance, inoxidizability, therefore is expected to be suitable as record Jie
The material of matter.The FePt phase has the order-disorder change temperature in 1573K, even if usually alloy is quenched from high temperature
Fire also due to quickly ordering reaction and have L10Structure.Also, FePt phase is used to use as super high-density recording medium
When material, it is desirable that develop the FePt particle for ordering of sening as an envoy to and consistently dispersed with the state of Magnetic isolation high density as far as possible and orientation
Technology.
In view of the foregoing, proposing is made using non-magnetic materials such as carbon with L10The FePt magnetic-particle magnetic of structure every
The granular texture thin magnetic film from obtained by is used as the side of the magnetic recording media of the next-generation hard disk using heat-assisted magnetic recording mode
Case.The granular texture thin magnetic film forms such as flowering structure: making magnetic-particle magnetic insulation each other by the intervention of namagnetic substance.
As particulate-type magnetic recording media and relative known document, patent document 1, patent document 2, patent document can be enumerated
3, patent document 4, patent document 5, patent document 6, patent document 7, patent document 8 etc..
Above-mentioned magnetic recording layer is constituted by the magnetic phase such as Fe-Pt alloy and by the non-magnetic phase that the magnetism is isolated, as non-
One of the material of magnetic phase, carbon are effective.Wherein graphite has crystal structure made of Laminated Graphite alkene piece, therefore graphite has
Have a two-dimensional directionality, i.e., with conduction is easy on the direction of piece surface level, be difficult to lead on the direction vertical with piece surface
Electricity.Therefore, if the orientation of graphite can be aligned, the electric current in sputtering can be stablized, so as to inhibit paradoxical discharge.
Usually using this magnetic recording layer of the film forming of the sputtering target made of sintered body, but pass through powder sintering, it is difficult to
It is aligned the orientation of the graphite in sintered body, as a result there are problems that desired stable sputtering characteristic cannot be obtained.
Existing technical literature
Patent document
Patent document 1: Japanese Unexamined Patent Publication 2000-306228 bulletin
Patent document 2: Japanese Unexamined Patent Publication 2000-311329 bulletin
Patent document 3: Japanese Unexamined Patent Publication 2008-59733 bulletin
Patent document 4: Japanese Unexamined Patent Publication 2008-169464 bulletin
Patent document 5: Japanese Unexamined Patent Publication 2012-102387 bulletin
Patent document 6: Japanese Unexamined Patent Publication 2011-208265 bulletin
Patent document 7: International Publication WO2012/086335
Patent document 8: Japanese Unexamined Patent Publication 2012-214874 bulletin
Summary of the invention
Problem to be solved by the invention
Project of the invention provides above-mentioned magnetic recording layer and is mutually isolated with by the magnetism by FePt based alloy etc. is magnetic
Non-magnetic phase is constituted, and the ferromagnetic material sputtering target for one of using material of the carbon (C) as non-magnetic phase, and provides inhibition
The ferromagnetic material sputtering target that as caused by paradoxical discharge powder generates when sputtering.
The means used to solve the problem
In order to solve the above problems, successfully to a certain extent by the orientation of the graphite in sintered body before the present inventor
It is aligned (Japanese Patent Application 2012-161563).It, will be as the magnetic Fe-Pt alloyed powder mutually used in order to which the orientation of graphite to be aligned
Formed flat, and it is effective that it, which is mixed with laminar graphite powder, but the partial size of Fe-Pt alloyed powder is thin and has
It is equably carried out flaky process and is difficult by porous structure.
Therefore, present inventor has performed further investigations, as a result obtain following discovery: controlled by using fine and close and partial size
Fe-Pt alloyed powder as the Fe-Pt alloyed powder before flaky process, can obtain and equably carry out flat processing
Fe-Pt alloyed powder.
And it was found that by this has equably been carried out flaky process Fe-Pt alloyed powder and thin slice graphite mixing,
It can be further improved the orientation of the graphite in sintered body, as a result, it is compared with the past, sputtering can be further suppressed
Paradoxical discharge, and the generation of powder can be further reduced.
Based on this discovery, the present invention is provided:
1) a kind of FePt base magnetic recording film formation sputtering target containing C, which is characterized in that in the section vertical with sputter face
Burnishing surface in, the average thickness of Fe-Pt alloy phase is 10 μm or more；
2) a kind of FePt base magnetic recording film formation sputtering target containing C, which is characterized in that in the section vertical with sputter face
Burnishing surface in, the average length of Fe-Pt alloy phase is 20 μm or more；
3) a kind of FePt base magnetic recording film formation sputtering target containing C, which is characterized in that in the section with sputter face level
Burnishing surface in, the average length of Fe-Pt alloy phase is 20 μm or more；
4) it is above-mentioned 1)~3) any one of described in sputtering target, which is characterized in that Pt content is 5 moles of % or more and 60 rubs
You are % or less；
5) it is above-mentioned 1)~4) any one of described in sputtering target, which is characterized in that C content is 10 moles of % or more and 70 rubs
You are % or less；
6) it is above-mentioned 1)~5) any one of described in sputtering target, which is characterized in that containing 0.5 mole of % or more and 10 rub
Your % is below to be selected from by one or more of B, Ru, Ag, Au, Cu group formed element as addition element；
7) it is above-mentioned 1)~6) any one of described in sputtering target, which is characterized in that containing selected from by oxide, nitride,
One or more of the group of carbide, carbonitride composition inorganic material is as added material；
8) a kind of manufacturing method of sputtering target, which is characterized in that Fe-Pt alloy is cut as chip, is then crushed
And carry out flaky process and obtain Fe-Pt alloy powder, then sheet powdered graphite and the Fe-Pt alloy powder are mixed
It closes, hot pressed sintering is carried out to the mixed-powder, then the sintered body is machined as target shape；
9) it is above-mentioned 8) described in sputtering target manufacturing method, which is characterized in that mixing B, Ru, Ag, Au, Cu selected from being made of
One or more of group metallic element powder；
10) it is above-mentioned 8) or 9) described in sputtering target manufacturing method, which is characterized in that mixing is selected from by oxide, nitridation
The powder of one or more of the group of object, carbide, carbonitride composition inorganic material.
Invention effect
The present invention relates to the magnetic recordings being made of the non-magnetic phase of the magnetic phase of Fe-Pt alloy etc. and the C being isolated from it etc.
Layer, which is formed, uses sputtering target, and has following excellent effect: can provide and inhibit the powder as caused by paradoxical discharge in sputtering
The ferromagnetic material sputtering target that grain generates.
Detailed description of the invention
[Fig. 1] is the laser microscope photo (photo for showing the section vertical with sputter face of target tissue of embodiment 1
It is upper: 1080 μm longitudinal, lateral 1450 μm of the visual field, under photo: 560 μm longitudinal, lateral 750 μm of the visual field).
[Fig. 2] is the laser microscope photo (photo with the section of sputter face level for showing the target tissue of embodiment 1
It is upper: 1080 μm longitudinal, lateral 1450 μm of the visual field, under photo: 560 μm longitudinal, lateral 750 μm of the visual field).
[Fig. 3] is the laser microscope photo (photo for showing the section vertical with sputter face of target tissue of embodiment 2
It is upper: 1080 μm longitudinal, lateral 1450 μm of the visual field, under photo: 560 μm longitudinal, lateral 750 μm of the visual field).
[Fig. 4] is the laser microscope photo (photo with the section of sputter face level for showing the target tissue of embodiment 2
It is upper: 1080 μm longitudinal, lateral 1450 μm of the visual field, under photo: 560 μm longitudinal, lateral 750 μm of the visual field).
[Fig. 5] is the laser microscope photo (photo for showing the section vertical with sputter face of target tissue of comparative example 1
It is upper: 1080 μm longitudinal, lateral 1450 μm of the visual field, under photo: 560 μm longitudinal, lateral 750 μm of the visual field).
[Fig. 6] is the laser microscope photo (photo with the section of sputter face level for showing the target tissue of comparative example 1
It is upper: 1080 μm longitudinal, lateral 1450 μm of the visual field, under photo: 560 μm longitudinal, lateral 750 μm of the visual field).
[Fig. 7] be C phase of the invention orientation alignment target vertical cross-section tissue schematic diagram (in figure, black part
Divide and correspond to C phase, white portion corresponds to alloy phase).
[Fig. 8] is to show the vertical cross-section of sputtering target of the invention and the schematic diagram of horizontal cross-section.
Specific embodiment
The present invention relates to have the C phase of the non-magnetic material in the Fe-Pt alloy phase of strong magnetic material according to along specific
The mode of orientation alignment disperses the sputtering target of the tissue (referring to Fig. 7).In this way, by being aligned the orientation of C phase along specific orientation,
The electric current in sputtering can be made to stablize, so as to inhibit paradoxical discharge.
Sputtering target of the invention is characterized in that the burnishing surface in the section vertical with sputter face (is finished based on polishing
Mirror finish face) in, the average thickness of Fe-Pt alloy phase is 10 μm or more.If the average thickness of Fe-Pt alloy phase is less than
10 μm, then since Fe-Pt alloy is easy cohesion each other, thus C phase is made to disperse and become difficult along specific orientation alignment.It is logical
Crossing makes 10 μm of average thickness of Fe-Pt alloy phase or more, can inhibit the mutual cohesion of Fe-Pt alloy, make C phase in target tissue
In it is evenly dispersed, and the orientation of C phase can be made to be aligned, so as to realize stable sputtering.
It should be noted that as shown in figure 8, " section vertical with sputter face " be equivalent to when hot pressing be pressurized
The vertical section in face.
The average thickness of the following Fe-Pt alloy phase for calculating vertical cross-section.
Firstly, fall into laterally, shoot in the visual field of longitudinal each 1000 μm~1500 μm of range any 3 positions with
The microscope photo in the vertical section of sputter face.At this point, adjusting the straight line relative to sputter face vertical direction, make itself and microscope
The longitudinal direction of photo is parallel.Then, straight line is drawn along the longitudinal of microscope photo in any 3 positions for each microscope photo.This
When, straight line is alternately through Fe-Pt alloy phase, C phase, the phase of other addition element.Then, by the straight line from beginning through mutually to this
The length of the line segment mutually terminated is defined as the thickness of phase, measures the thickness of each phase of Fe-Pt alloy phase, and calculating locates 3
Position × microscope photo 3 is opened=amounts to the average value of the measured value of 9 positions.
It should be noted that cannot ensure to be enough to calculate in the case where the visual field of microscope photo is narrower than above range
The parameter of average thickness, on the other hand, in the case where bigger than above range, the measurement of the length of every phase is become difficult, therefore
Preferable field of view is 1000 μm~1500 μm.
In addition, sputtering target of the invention is characterized in that, the burnishing surface in the section vertical with sputter face is (smart based on polishing
The mirror finish face of processing) in, the average length of Fe-Pt alloy phase is 20 μm or more.Although Fe-Pt alloy is preparatory before mixing
Flattening or sheet processing are carried out, but by having a degree of length in the longitudinal direction, makes C phase perpendicular to sputter face
Direction on stratiform easy to form.
Preferably, in the burnishing surface in the section vertical with sputter face, the average thickness of Fe-Pt alloy phase be 10 μm with
On, and the average length of the alloy phase is 30 μm or more.In addition, if the average thickness of Fe-Pt alloy phase is blocked up or average
Length is too long, then is 100 μm hereinafter, or average length is 400 it is advantageous to average thickness because becoming difficult orientation alignment
μm or less.
The average length of the following Fe-Pt alloy phase for calculating vertical cross-section.
Firstly, shot in falling into the longitudinally, laterally visual field of each 1000 μm~1500 μm of range any 3 positions with
The microscope photo in the vertical section of sputter face.At this point, adjusting the straight line relative to sputter face vertical direction, make itself and microscope
The longitudinal direction of photo is parallel.Then, straight line is drawn along the lateral of microscope photo in any 3 positions for each microscope photo.This
When, straight line is alternately through Fe-Pt alloy phase, C phase, the phase of other addition element.Then, by the straight line from beginning through mutually to this
The length of the line segment mutually terminated is defined as the length of phase, measures the length of each phase of Fe-Pt alloy phase, and calculating locates 3
Position × microscope photo 3 is opened=amounts to the average value of the measured value of 9 positions.
It should be noted that cannot ensure to be enough to calculate in the case where the visual field of microscope photo is narrower than above range
The parameter of average length, on the other hand, in the case where bigger than above range, the measurement of the length of every phase is become difficult, therefore
Preferable field of view is 1000 μm~1500 μm.
In addition, sputtering target of the invention is characterized in that, the burnishing surface in the section with sputter face level is (smart based on polishing
The mirror finish face of processing) in, the average length of Fe-Pt alloy phase is 20 μm or more.Mutually there is certain journey by Fe-Pt alloy
The length and width of degree makes C phase stratiform easy to form on the direction perpendicular to sputter face.
It is highly preferred that in the burnishing surface in the section vertical with sputter face, the average thickness of Fe-Pt alloy phase be 20 μm with
On and/or the average length of the alloy phase be 20 μm or more, and in the burnishing surface in the section with sputter face level, Fe-Pt
The average length of alloy phase is 20 μm or more.
It should be noted that as shown in figure 8, " section with sputter face level " be equivalent in hot pressing be pressurized
Face.
The average length of the following Fe-Pt alloy phase for calculating horizontal cross-section.
Firstly, shot in falling into the longitudinally, laterally visual field of each 1000 μm~1500 μm of range any 3 positions with
The microscope photo in the section of sputter face level.At this point, since Fe-Pt alloy does not have the direction of 2 dimensions mutually in horizontal cross-section
Property, thus can in any direction on shot.Then, each microscope photo is shone in any 3 positions along microscope
The lateral of piece draws straight line.At this point, straight line is alternately through Fe-Pt alloy phase, C phase, the phase of other addition element.Then, this is straight
Line is mutually defined as the length of phase from beginning through to the length of the line segment mutually terminated, measures the length of each phase of Fe-Pt alloy phase
Degree calculates 3 positions × microscope photo 3 is opened=that locate and amounts to the average value of the measured value of 9 positions.
It should be noted that cannot ensure to be enough to calculate in the case where the visual field of microscope photo is narrower than above range
The parameter of average length, on the other hand, in the case where bigger than above range, the measurement of the length of every phase is become difficult, therefore
Preferable field of view is 1000 μm~1500 μm.
The preferred Pt content of sputtering target of the invention is 5 moles of % or more and 60 mole of % hereinafter, rest part is Fe and C.
This is because desired magnetic characteristic cannot be obtained sometimes if Pt content is lower than 5 moles of % or more than 60 moles %.
In addition, for sputtering target of the invention, preferably C content be 10 moles of % or more and 70 mole of % hereinafter, its
Remaining part is divided into Fe and Pt.This is because desired magnetic characteristic cannot be obtained sometimes when C content is lower than 10 moles of %, it is another
Aspect, when C content is more than 70 moles of %, C agglomerates, so as to cause powder increase.
In addition, in order to improve magnetic characteristic, sputtering target of the invention preferably comprises 0.5 mole of % or more and 10 mole of % or less
Selected from by one or more of B, Ru, Ag, Au, Cu group formed element as addition element.In addition, by addition selected from by
Oxide, nitride, carbide, carbonitride composition one or more of group inorganic material as added material, can be with
Further increase magnetic characteristic.
The manufacturing method of sputtering target of the invention is illustrated.
Firstly, melting and casting Fe raw material and Pt raw material, to make Fe-Pt alloy pig, and will using general lathe etc.
Fe-Pt alloy chip is made in it.At this point, it is preferred that approach when cutting is 0.1mm~0.3mm.In addition, the Fe raw material used and
Pt raw material can be arbitrary shape, as long as it is can be with the shape of induction heating.
The reasons why alloy is made by melting and casting is, in the case where sintered alloy is made in Fe powder and Pt powder, is formed
Porous structure, Fe-Pt alloyed powder is pulverized in aftermentioned flaky process, as a result forms the small alloyed powder of partial size.
It can be with the ratio for forming suitably adjusting Fe raw material and Pt raw material of as expected Fe-Pt alloy.In addition,
In the case where the metal powder for adding B, Ru, Ag, Au, Cu etc., preferably added while making Fe-Pt alloy pig.
Then, by the chip of Fe-Pt alloy using Blang's horizontal pulverizer crush until by sieve pore be 150 μm~
400 μm of sieve.Then, it is classified using 63 μm of purposes sieve, uses residue on sieve as raw material.If Fe-Pt is closed
The partial size of bronze is too small, then alloyed powder is passed through between crushing medium in subsequent process, it is difficult to carry out equably flattening
Processing, therefore not preferably.
Then, it using medium stirring mill, crushes as flat or laminar (flaky process).When use has the tank of 5L
When the medium stirring mill of capacity, it is preferable that use the yttria stabilized zirconia pearl of diameter 3mm~7mm as crushing medium,
It carries out handling for about 2 hours~about 8 hours under the revolving speed of 300rpm.But the present invention is not limited to this conditions, and can be used and appoint
Where method, as long as its processing capacity for being recognized as that the degree of being identical with this can be obtained.
By above-mentioned pulverizing process and flaky process, partial size can be obtained as 1 μm or more and 500 μm or less, average grain
The fine and close Fe-Pt alloy powder that diameter is 50 μm~100 μm.
For C raw material powder, it is preferable to use flat or laminar graphite or thin slice graphite (number of plies of graphite is few
Graphite).Thin slice graphite and common graphite-phase ratio have superior electric conductivity, therefore to inhibition paradoxical discharge and reduce powder
Grain is effective.It is preferable to use partial size be 0.5 μm or more and 30 μm or less, average thickness is 0.5 μm or more and 30 μm of C below
Raw material powder.If C raw material is meticulous, C raw material aggregates with one another, therefore not preferably, when C raw material is excessive, C raw material becomes itself
The reason of paradoxical discharge, therefore not preferably.
Then, weigh above-mentioned raw materials powder with obtain it is desired form, the use of mortar or sieve pore is 150 μm~500 μm
Sieve mixes these powder.
In inorganic matters such as metal powders or oxide, nitride, carbide, carbonitride such as addition B, Ru, Ag, Au, Cu
In the case where material, it can be mixed in this stage.It is preferable to use 0.5 μm of partial size or more and 30 μm of these metal powders below
End or powdered inorganic material.If raw material is meticulous, raw material aggregates with one another, therefore not preferably, if raw material is excessive, raw material is certainly
Body becomes the reason of paradoxical discharge, therefore not preferably.
As described above, by using the Fe-Pt alloyed powder and thin slice graphite that have equably carried out flaky process, and
The aforementioned metal powder or powdered inorganic material being added as needed are compared with the past as raw material powder, can further mention
The orientation of C phase of the height in the target made of sintered body.
Then, mixed powder is filled into carbon molding jig, is formed, is sintered by the hot pressing that uniaxial direction is pressurizeed.?
When the hot pressing of such single shaft direction pressurization, C, which hands down, is specifically orientated alignment.
Holding temperature when sintering depends on the composition of sputtering target, is in most cases 800 DEG C~1600 DEG C of temperature model
It encloses.In addition, as needed, hot isostatic pressing processing can be carried out to the sintered body taken out from hot press.Hot isostatic pressing processing for
The density for improving sintered body is effective.Hot isostatic pressing process when holdings temperature depending on sintered body composition, in most cases for
800 DEG C~1600 DEG C of temperature range.In addition, pressure is set as 100Mpa or more.By will in this way be obtained using lathe
Sintered body is processed into desired shape, can make sputtering target of the invention.
Embodiment
Hereinafter, being illustrated based on embodiment and comparative example.It should be noted that the present embodiment is only illustrative, sheet
Invention is not by this any restrictions.That is, the present invention is only limited by the claims, be included in embodiment contained in the present invention with
Outer various modifications.
(embodiment 1)
Firstly, by vacuum melting casting by Fe raw material and Pt raw material melting, to obtain columned group of about φ 150
At than the alloy pig for Fe-50Pt (atom %).Then, the surface film oxide of the alloy pig of acquisition is removed, is then set
It sets in universal lathe, is cut with the approach of 0.3mm, to make Fe-Pt alloy chip.
Then, the chip of Fe-Pt alloy is crushed using Blang's horizontal pulverizer until being 150 μm by sieve pore
Then sieve is 63 μm using sieve pore and screens out micro mist.Then, the medium that Fe-Pt comminuted powder investment tankage size is 5L is stirred
Mill uses the yttria stabilized zirconia pearl of diameter 5mm handle within 4 hours as crushing medium, to make densification
Sheet Fe-Pt alloy powder.
In order to investigate the densification sheet Fe-Pt alloy powder average grain diameter, the wet type manufactured using Ku Chang company
Particle size distribution analysis instrument, and isopropanol is used to be measured as dispersion solvent, as a result fine and close Fe-Pt alloy powder is flat
Equal partial size is 85 μm.
Then, it is ready to pass through the sheet that the average grain diameter after air current classifying method separates the particle of minor diameter is 25.5 μm
Powdered graphite, it is 400 μm that the fine and close Fe-Pt alloy powder and sheet powdered graphite by above-mentioned acquisition, which is used sieve pore,
Sieve mixed so that ratio of components be (Fe-50Pt) -40C (atom %), fill it into carbon molding jig, and carry out hot pressing.
The condition of hot pressing are as follows: vacuum atmosphere, is kept for 1400 DEG C of temperature, the retention time 2 is small by 300 DEG C/h of heating rate
When, to the pressure for keeping terminating application 30MPa since heating.Make products therefrom natural as former state in chamber after holding
It is cooling.
Then, hot isostatic pressing processing is carried out to the sintered body taken out from the mold of hot press.The item of hot isostatic pressing processing
Part are as follows: 300 DEG C/h of heating rate, 1100 DEG C of temperature of holding, the retention time 2 hours, by the gas of Ar gas since heating
Pressure increases gradually, applies the pressure of 150MPa during being kept for 1100 DEG C.Make products therefrom original sample in furnace after holding
Natural cooling.
Then, the end of the sintered body of acquisition is cut, to relative to sputter face horizontal plane and vertical cross-section throw
Light, in its tissue of laser capture microdissection microscopic observation.Then, the optional position in tissue surface is with 1080 μm longitudinal, lateral
1450 μm of visual field sizes and 560 μm longitudinal, lateral 750 μm of visual field sizes shoot organization chart picture.The image of shooting is respectively such as
Shown in Fig. 1, Fig. 2.White portion in structure observation image is the part corresponding to Fe-Pt phase.On the other hand, black portions are
Part corresponding to C phase.
It is measured using the average thickness of the Fe-Pt phase in the organization chart picture pair section vertical with sputter face, as a result
It is 11.9 μm.In addition, to the average length of the Fe-Pt phase on direction parallel with sputter face in the vertical section of sputter face into
Row measurement, result are 29.7 μm.In addition, being measured to the average length with the Fe-Pt phase in the section of sputter face level, tie
Fruit is 27.6 μm.
It then, is diameter 180.0mm by the sintered body machining with lathe, the shape of thickness 5.0mm is then fitted into
In magnetic control sputtering device (the C-3010 sputtering system of Canon Anelva manufacture) and sputtered.The condition of sputtering are as follows: defeated
Enter power 1kW, Ar atmospheric pressure 1.7Pa, after the pre-sputtering for implementing 2kWh, carries out 20 on the silicon substrate with 4 inch diameters
Second film forming.Then using Superficial Foreign Body check device (manufacture of Surfscan 6420, KLA-Tencor company) measurement on substrate
The number of the powder of attachment, result are 103, are substantially reduced compared with aftermentioned comparative example 1.The above knot is summarized in table 1
Fruit.
Table 1
(embodiment 2)
It is dissolved firstly, Fe raw material and Pt raw material are cast by vacuum melting, to obtain columned group of about φ 150
At than the alloy pig for Fe-50Pt (atom %).Then, the surface film oxide of the alloy pig of acquisition is removed, is then set
It sets in universal lathe, is cut with the approach of 0.1mm, to make Fe-Pt alloy chip.
Then, the chip of Fe-Pt alloy is crushed using Blang's horizontal pulverizer until being 150 μm by sieve pore
Then sieve is 63 μm using sieve pore and screens out micro mist.Then, the medium stirring mill for being 5L by Fe-Pt chip investment tankage size,
The yttria stabilized zirconia pearl of diameter 5mm is used handle within 4 hours as crushing medium, to make the thin of densification
Piece Fe-Pt alloy powder.
In order to investigate this densification sheet Fe-Pt alloy powder average grain diameter, manufactured using Ku Chang company wet
Formula particle size distribution analysis instrument, and isopropanol is used to be measured as dispersing agent, as a result fine and close sheet Fe-Pt alloyed powder
The average grain diameter at end is 80 μm.
Then, it is ready to pass through the sheet that the average grain diameter after air current classifying method separates the particle of minor diameter is 25.5 μm
Powdered graphite, it is 400 μm that the fine and close Fe-Pt alloy powder and sheet powdered graphite by above-mentioned acquisition, which is used sieve pore,
Sieve mixing so that ratio of components be (Fe-50Pt) -40C (atom %), fill it into carbon molding jig, and carry out hot pressing.
The condition of hot pressing are as follows: vacuum atmosphere, is kept for 1400 DEG C of temperature, the retention time 2 is small by 300 DEG C/h of heating rate
When, to the pressure for keeping terminating application 30MPa since heating.Make products therefrom natural as former state in chamber after holding
It is cooling.
Then, hot isostatic pressing processing is carried out to the sintered body taken out from the mold of hot press.The item of hot isostatic pressing processing
Part are as follows: 300 DEG C/h of heating rate, 1100 DEG C of temperature of holding, the retention time 2 hours, by the gas of Ar gas since heating
Pressure increases gradually, applies the pressure of 150MPa during being kept for 1100 DEG C.Make products therefrom original sample in furnace after holding
Natural cooling.
Then, the end of the sintered body of acquisition is cut, to relative to sputter face horizontal plane and vertical cross-section throw
Light, in its tissue of laser capture microdissection microscopic observation.Then, the optional position in tissue surface is with 1080 μm longitudinal, lateral
1450 μm of visual field sizes and 560 μm longitudinal, lateral 750 μm of visual field sizes shoot organization chart picture.The image of shooting is respectively such as
Shown in Fig. 3, Fig. 4.The white portion of structure observation image is the part corresponding to Fe-Pt phase.On the other hand, black portions are pair
It should be in the part of C phase.
It is measured using the average thickness of the Fe-Pt phase in the organization chart picture pair section vertical with sputter face, as a result
It is 12.3 μm.In addition, to the average length of the Fe-Pt phase on direction parallel with sputter face in the vertical section of sputter face into
Row measurement, result are 37.1 μm.In addition, being measured to the average length with the Fe-Pt phase in the section of sputter face level, tie
Fruit is 31.9 μm.
It then, is diameter 180.0mm by the sintered body machining with lathe, the shape of thickness 5.0mm is then fitted into
In magnetic control sputtering device (the C-3010 sputtering system of Canon Anelva manufacture) and sputtered.The condition of sputtering are as follows: defeated
Enter power 1kW, Ar atmospheric pressure 1.7Pa, after the pre-sputtering for implementing 2kWh, carries out 20 on the silicon substrate with 4 inch diameters
Second film forming.Then using Superficial Foreign Body check device (manufacture of Surfscan 6420, KLA-Tencor company) measurement on substrate
The number of the powder of attachment, result are 76, are substantially reduced compared with aftermentioned comparative example 1.It is equally summarized in table 1 above
As a result.
(comparative example 1)
Firstly, preparing as 3 μm of average grain diameter of Fe powder of raw material powder and 3 μm of average grain diameter of Pt powder to make group
At than mix within 2 hours using mortar, being then heated to 800 DEG C in an inert atmosphere for Fe-50Pt (atom %), thus
Make its alloying.Then, it is enclosed to capacity together with the yttria stabilized zirconia pearl as the diameter 5mm of crushing medium
To carry out crushing for 4 hours at 300 rpm in 5 liters of medium stirring mills, to obtain Fe-Pt alloy powder.
Then, it is ready to pass through the sheet that the average grain diameter after air current classifying method separates the particle of minor diameter is 25.5 μm
Powdered graphite will be mixed by the Fe-Pt alloy powder of above-mentioned acquisition and sheet powdered graphite using the sieve that sieve pore is 400 μm
So that ratio of components is (Fe-50Pt) -40C (atom %), fill it into carbon molding jig, and carry out hot pressing.
The condition of hot pressing are as follows: vacuum atmosphere, is kept for 1400 DEG C of temperature, the retention time 2 is small by 300 DEG C/h of heating rate
When, to the pressure for keeping terminating application 30MPa since heating.Make products therefrom natural as former state in chamber after holding
It is cooling.
Then, hot isostatic pressing processing is carried out to the sintered body taken out from the mold of hot press.The item of hot isostatic pressing processing
Part are as follows: 300 DEG C/h of heating rate, 1100 DEG C of temperature of holding, the retention time 2 hours, by the gas of Ar gas since heating
Pressure increases gradually, applies the pressure of 150MPa during being kept for 1100 DEG C.Make products therefrom original sample in furnace after holding
Natural cooling.
Then, the end of the sintered body of acquisition is cut, to relative to sputter face horizontal plane and vertical cross-section throw
Light, in its tissue of laser capture microdissection microscopic observation.Then, the optional position in tissue surface is with 1080 μm longitudinal, lateral
1450 μm of visual field sizes and 560 μm longitudinal, lateral 750 μm of visual field sizes shoot organization chart picture.The image of shooting is respectively such as
Shown in Fig. 5, Fig. 6.The white portion of structure observation image is the part corresponding to Fe-Pt phase.On the other hand, black portions are pair
It should be in the part of C phase.
It is measured using the average thickness of the Fe-Pt phase in the organization chart picture pair section vertical with sputter face, as a result
It is 4.4 μm.In addition, to the average length of the Fe-Pt phase on direction parallel with sputter face in the vertical section of sputter face into
Row measurement, result are 14.3 μm.In addition, being measured to the average length with the Fe-Pt phase in the section of sputter face level, tie
Fruit is 9.2 μm.
It then, is diameter 180.0mm by the sintered body machining with lathe, the shape of thickness 5.0mm is then fitted into
In magnetic control sputtering device (the C-3010 sputtering system of Canon Anelva manufacture) and sputtered.The condition of sputtering are as follows: defeated
Enter power 1kW, Ar atmospheric pressure 1.7Pa, after the pre-sputtering for implementing 2kWh, carries out 20 on the silicon substrate with 4 inch diameters
Second film forming.Then using Superficial Foreign Body check device (manufacture of Surfscan 6420, KLA-Tencor company) measurement on substrate
The number of the particle of attachment, as a result up to 244.Equally result above is summarized in table 1.
Industrial applicability
The present invention, which provides, to be had in Fe-Pt alloy phase as the C phase of non-magnetic material according to along specific orientation alignment
The sputtering target of tissue that disperses of mode.By being aligned the orientation of C phase along specific orientation, there is following excellent effect: can be with
Stablize the electric current in sputtering, so as to inhibit paradoxical discharge.The present invention for magnetic recording media magnetic film, especially
The film forming for being corpuscular magnetic recording layer with ferromagnetic material sputtering target is useful.
Claims (9)
1. a kind of FePt base magnetic recording film formation sputtering target containing C, which is characterized in that the throwing in the section vertical with sputter face
In smooth surface, the average thickness of Fe-Pt alloy phase is 10 μm or more and 100 μm hereinafter, the average length of Fe-Pt alloy phase is 20 μm
Above and 400 μm hereinafter, C phase is dispersed in the way of along specific orientation alignment.
2. the FePt base magnetic recording film formation sputtering target containing C as described in claim 1, which is characterized in that with sputter face
In the burnishing surface in horizontal section, the average length of Fe-Pt alloy phase is 20 μm or more.
3. sputtering target according to claim 1 or 2, which is characterized in that Pt content be 5 moles of % or more and 60 mole of % with
Under.
4. sputtering target according to claim 1 or 2, which is characterized in that C content be 10 moles of % or more and 70 mole of % with
Under.
5. sputtering target according to claim 1 or 2, which is characterized in that contain 0.5 mole of % or more and 10 mole of % or less
Selected from by one or more of B, Ru, Ag, Au, Cu group formed element as addition element.
6. sputtering target according to claim 1 or 2, which is characterized in that containing selected from by oxide, nitride, carbide,
One or more of the group of carbonitride composition inorganic material is as added material.
7. a kind of manufacturing method of sputtering target, which is characterized in that cut Fe-Pt alloy for chip, then crushed and gone forward side by side
Row flaky process and obtain Fe-Pt alloy powder, then sheet powdered graphite is mixed with the Fe-Pt alloy powder, it is right
The mixed-powder is sintered by the hot pressing of uniaxial direction pressurization, and then the sintered body is machined as target shape.
8. the manufacturing method of sputtering target according to claim 7, which is characterized in that mixing is selected from by B, Ru, Ag, Au, Cu
The powder of one or more of group of composition addition element.
9. the manufacturing method of sputtering target according to claim 7 or 8, which is characterized in that mixing is selected from by oxide, nitridation
The powder of one or more of the group of object, carbide, carbonitride composition inorganic material.
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| CN102087858A (en) * | 2010-11-26 | 2011-06-08 | 山西师范大学 | Gradient composite magnetic recording media and preparation method thereof |
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| US20070189916A1 (en) * | 2002-07-23 | 2007-08-16 | Heraeus Incorporated | Sputtering targets and methods for fabricating sputtering targets having multiple materials |
| KR100470151B1 (en) * | 2002-10-29 | 2005-02-05 | 한국과학기술원 | HIGH-DENSITY MAGNETIC RECORDING MEDIA USING FePtC FILM AND MANUFACTURING METHOD THEREOF |
| JP5590322B2 (en) * | 2010-11-12 | 2014-09-17 | 三菱マテリアル株式会社 | Sputtering target for forming a magnetic recording medium film and method for producing the same |
| JP5290468B2 (en) * | 2010-12-20 | 2013-09-18 | Ｊｘ日鉱日石金属株式会社 | Fe-Pt sputtering target in which C particles are dispersed |
| JP5041262B2 (en) * | 2011-01-31 | 2012-10-03 | 三菱マテリアル株式会社 | Sputtering target for forming a magnetic recording medium film and method for producing the same |
| JP5912559B2 (en) * | 2011-03-30 | 2016-04-27 | 田中貴金属工業株式会社 | Method for producing FePt-C sputtering target |
| JP5301751B1 (en) * | 2011-09-26 | 2013-09-25 | Ｊｘ日鉱日石金属株式会社 | Fe-Pt-C sputtering target |
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| TW201531575A (en) | 2015-08-16 |
| MY191633A (en) | 2022-07-04 |
| CN109943814B (en) | 2021-04-20 |
| JP6484276B2 (en) | 2019-03-13 |
| JP2017197840A (en) | 2017-11-02 |
| WO2015076190A1 (en) | 2015-05-28 |
| SG11201602163YA (en) | 2016-04-28 |
| CN109943814A (en) | 2019-06-28 |
| CN105793465A (en) | 2016-07-20 |
| JP6125661B2 (en) | 2017-05-17 |
| JPWO2015076190A1 (en) | 2017-03-16 |
| MY177997A (en) | 2020-09-29 |
| TWI642799B (en) | 2018-12-01 |
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