CN103380458B - Magnetic recording non-retentive alloy, sputtering target material and magnetic recording media - Google Patents
Magnetic recording non-retentive alloy, sputtering target material and magnetic recording media Download PDFInfo
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- CN103380458B CN103380458B CN201280008677.9A CN201280008677A CN103380458B CN 103380458 B CN103380458 B CN 103380458B CN 201280008677 A CN201280008677 A CN 201280008677A CN 103380458 B CN103380458 B CN 103380458B
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- 239000000463 material Substances 0.000 title claims description 26
- 238000005477 sputtering target Methods 0.000 title claims description 16
- 229910052802 copper Inorganic materials 0.000 claims abstract description 9
- 229910052803 cobalt Inorganic materials 0.000 claims abstract description 8
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 7
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 7
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 7
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 7
- 229910052796 boron Inorganic materials 0.000 claims abstract description 6
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
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- 238000005260 corrosion Methods 0.000 abstract description 23
- 230000004907 flux Effects 0.000 description 25
- 239000010408 film Substances 0.000 description 17
- 238000007792 addition Methods 0.000 description 8
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- 238000004544 sputter deposition Methods 0.000 description 7
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- 238000001755 magnetron sputter deposition Methods 0.000 description 5
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Abstract
The present invention provides a kind of and comprises in terms of at.%: (A) of more than 0.5% is selected from the one kind or two or more of the element in Ta, Nb and V；(B) of more than 0.5% is selected from the one kind or two or more of the element in Cr, Mo and W；0～(C) element in Ti, Zr and Hf one kind or two or more of 5%；0～a kind or 2 kinds of (D) element in Ni and Mn of 30%；0～a kind or 2 kinds of (E) element in Al and Cu of 5%；0～(F) element in Si, Ge, P, B and C one kind or two or more of 10%；The magnetic recording non-retentive alloy that remainder is made up of Co and Fe and inevitable impurity.The ratio of Fe: Co of this alloy is 10: 90～70: 30, and total amount is described alloy the 10～30% of (A) group element, (B) group element and (C) group element.The amorphism of the alloy of the present invention, hardness and excellent corrosion resistance, be suitable for use as the non-retentive alloy of perpendicular magnetic recording medium.
Description
Related application
The application advocates priority based on Japanese patent application filed in 16 days February in 2011 2011-30562, will
Its whole disclosure is by referring to including in this specification.
Technical field
The present invention relates to the Co system magnetic recording non-retentive alloy used as the soft ferromagnetic layer in perpendicular magnetic recording medium
And sputtering target material and possess the magnetic recording media of this kind of soft ferromagnetic layer.
Background technology
In recent years, the progress of perpendicular magnetic recording is notable, and in order to realize the high capacity of driver, magnetic recording densityization is
In the middle of advancing, in will be carried out the face popularized than ever, the more highdensity perpendicular magnetic recording of return to zero is practical
Change.Here, so-called perpendicular magnetic recording, is relative to the medium side in the magnetic film of perpendicular magnetic recording medium by easy magnetizing axis
The mode that vertical direction orientation ground is formed, the method being adapted for densification.In this return to zero, improve note as having
The magnetic recording layer of record density and the multilayer recording medium in soft ferromagnetic layer and intermediate layer are developed.And, in this magnetic recording layer
Generally use CoCrPt-SiO2It it is alloy.
On the other hand, for soft magnetic film layer, Japanese Unexamined Patent Publication 2008-299905 publication (patent documentation 1), Japan spy
Open in 2008-189996 publication (patent documentation 2), proposed to change as substrate with the addition of using the soft magnetism element of Co or Fe
Kind non-crystalline Zr, Hf, the alloy of Ta, Nb and B.High saturation magnetic flux is required in the soft magnetic film layer of this perpendicular magnetic recording medium
Density, high amorphism and highly corrosion resistant.
It addition, as the soft ferromagnetic layer of 2 layers of record medium, proposed the soft magnetic film of Fe-Co-B based compound, such as,
As disclosed in Japanese Unexamined Patent Publication 2004-346423 publication (patent documentation 3), proposed in section microstructure not
There is the Fe-Co-B target of below a diameter of 30 μm of the maximum inscribed circle can described in the region of boride layer.
In the film forming of above-mentioned soft magnetic film, generally use magnetron sputtering method.This magnetron sputtering method refers to, at target
Distributed magnet behind, makes flux leakage on the surface of target, by plasma confinement is permissible in this leakage magnetic flux region
Realize the sputtering method of constraint film forming.This magnetron sputtering method is characterised by, the sputtering surface at target makes flux leakage, therefore exists
In the case of the permeability height of target self, it is difficult to the sputtering surface at target forms foot required for magnetron sputtering method
Enough leakage magnetic flux.So, propose patent documentation 3 for the requirement of permeability that must reduce target self as far as possible.
But, the limit of the thickness of above-mentioned target goods is about 5mm, if making it thicker than this thickness, would not produce
Raw enough leakage magnetic flux, therefore have the problem that cannot be carried out normal magnetron sputtering.Further, since require to exist at this target
It is high magnetic flux density during film forming, the most preferably have employed the material of Fe substrate, but in the case of being somebody's turn to do, deposit in terms of corrosion resistance
In problem, it addition, cause paradoxical discharge to cause sputtering in oxidation section when having because of the oxidation of target the quality of film to deteriorate, sputter
Bad situation.
In order to solve this problem, in Japanese Unexamined Patent Publication 2007-284741 publication (patent documentation 4), reported and do not made magnetic
Improve to deterioration in characteristics the making of the soft magnetism target of corrosion resistance, but excellent amorphism is silent on.
Summary of the invention
The present inventor etc. this time find, utilize the interpolation of (A) group element in Ta, Nb and V can improve amorphism,
It addition, utilize the interpolation of (B) group element in Cr, Mo and W can improve hardness, utilize (C) in Ti, Zr and Hf
The interpolation of group element may insure that amorphism, and the element that these (A) groups, (B) group and (C) organize is in terms of corrosion resistance improvement
The most effective.Thus, it is possible to the magnetic recording non-retentive alloy that amorphism, corrosion resistance, hardness are excellent is provided.And, non-
In terms of reducing noise effectively, in terms of impact resistance effectively, corrosion resistance is effective in terms of the filming of carbon film for hardness for crystalline substance.
So, it is an object of the invention to, it is provided that the perpendicular magnetic recording medium of amorphism, hardness and excellent corrosion resistance
With non-retentive alloy and for making the sputtering target material of the thin film of this alloy.
A mode according to the present invention, it is provided that a kind of magnetic recording non-retentive alloy, is to comprise in terms of at.%:
(A) of more than 0.5% is selected from the one kind or two or more of the element in Ta, Nb and V；
(B) of more than 0.5% is selected from the one kind or two or more of the element in Cr, Mo and W；
0～(C) element in Ti, Zr and Hf one kind or two or more of 5%；
0～a kind or 2 kinds of (D) element in Ni and Mn of 30%；
0～a kind or 2 kinds of (E) element in Al and Cu of 5%；
0～(F) element in Si, Ge, P, B and C one kind or two or more of 10%；Remainder by Co and Fe with
And the magnetic recording non-retentive alloy that inevitably impurity is constituted,
The ratio of Fe: Co is 10: 90～70: 30, and the total amount of (A) group element, (B) group element and (C) group element is institute
State the 10～30% of alloy.
Another mode according to the present invention, it is provided that the sputtering target being made up of the magnetic recording non-retentive alloy of the present invention
Material.
Another mode according to the present invention, it is provided that possess the soft magnetism being made up of the magnetic recording non-retentive alloy of the present invention
The magnetic recording media of property layer.
Detailed description of the invention
Hereinafter the present invention is specifically described.As long as no particularly expressing, in this specification, " % " refers to at%.
The magnetic recording non-retentive alloy of the present invention, in terms of at.%, comprises (A) choosing of (comprising) more than 0.5%
Element in Ta, Nb and V one kind or two or more；1 kind or 2 kinds of (B) of more than 0.5% element in Cr, Mo and W
Above；0～(C) element in Ti, Zr and Hf one kind or two or more of 5%；0～30% (D) in Ni and Mn
1 kind or 2 kinds of element；0～a kind or 2 kinds of (E) element in Al and Cu of 5%；0～10% (F) selected from Si,
Element in Ge, P, B and C one kind or two or more, remainder by Co and Fe and inevitably impurity constitute, preferably by
These elements and inevitably impurity substantially constitute (consisting essentially of), the most only by this
A little elements and inevitably impurity constitute (consisting of).The ratio of Fe: Co of the alloy of the present invention is 10: 90～70:
30, and total amount is alloy the 10～30% of (A) group element, (B) group element and (C) group element.
Fe and Co is soft magnetism constitution element, with 10: 90～70: 30 Fe: Co ratio be contained in alloy.Fe's Yu Co
Ratio is to ensure that soft magnetism and the parameter producing a very large impact saturation flux density, amorphism, hardness and corrosion resistance, special
Not being that then saturation flux density is abundant not if making the ratio of Fe: Co less than 10, additionally if it exceeds 70, then corrosion resistance is bad
Change.
(A) group element be in Ta, Nb and V one kind or two or more, improve the element of amorphism and hardness, closing
Gold comprises more than 0.5at.%, preferably comprises 2～20at.%, more preferably comprise 4～15at.%.If it is not enough
0.5at.%, the most above-mentioned to improve effect the most abundant.
(B) group element be in Cr, Mo and W one kind or two or more, improve the element of amorphism and corrosion resistance,
Comprise more than 0.5at.% in the alloy, preferably comprise 1～20at.%, more preferably comprise 2～10at.%.If it is not enough
0.5at.%, the most above-mentioned to improve effect the most abundant.
(C) group element be in Ti, Zr and Hf one kind or two or more, improve non-crystalline element, in the alloy
Comprise 0～5at.%, preferably comprise 2～4at.%.If it exceeds 5at.%, then cannot obtain saturation flux density fully.
(A) total amount of group element, (B) group element and (C) group element is set to the 10～30at.% of alloy.(A) group element,
(B) group element and (C) group element are all the elements improving amorphism and corrosion resistance, if but the total amount of these elements be less than
10at.%, then its effect is abundant not, on the other hand, if it exceeds 30%, then cannot obtain saturation flux density fully.
(D) group element be a kind in Ni and Mn or 2 kinds, the arbitrary element that adjusts saturation flux density, at alloy
In comprise 0～30at.%, preferably comprise more than 0% and for below 30at.%, more preferably comprise below 10at.%, further
Preferably comprise 1～5at.%.If in the range of these, then it is prone to obtain saturation flux density fully.
(E) group element be a kind in Al and Cu or 2 kinds, the arbitrary element that improves corrosion resistance, wrap in the alloy
Containing 0～5at.%, preferably comprise more than 0% and for below 5at.%, more preferably comprise 1～4at.%.If in these scopes
In, then amorphism is difficult to reduce.
(F) group element be in Si, Ge, P, B and C one kind or two or more, improve non-crystalline arbitrary element, bag
Containing 0～10at.%, preferably comprise more than 0% and for below 10at.%, more preferably comprise 1～8at.%.If at these models
In enclosing, then above-mentioned effect of improving can not be made to prevent the reduction of saturation flux density saturatedly.
The sputtering target material of the present invention is made up of above-mentioned magnetic recording non-retentive alloy.The thickness of sputtering target material limits the most especially
Fixed, even the thickness more than 5mm, it is also possible to sputter normally, preferably more than 7mm.By using this kind of present invention
Sputtering target material sputter, it is possible to manufacture possess the soft ferromagnetic layer being made up of above-mentioned magnetic recording non-retentive alloy magnetic note
Recording medium.
Embodiment
Hereinafter, utilize embodiment that the alloy of the present invention is specifically described.
As a rule, the Seed Layer in perpendicular magnetic recording medium can be by the sputtering target of sputtering with its composition identical component
Material, on glass substrate etc., film forming prepares.Here, by sputtering the thin film of film forming by chilling.As the confession in the present invention
Test material, uses the chilling strip utilizing the quenching apparatus of mono-roller type to make.This is to utilize liquid chilling thin easily
Bring the impact on various characteristics caused by heterogeneity of the strip of film forming by sputtering in evaluation reality.
The manufacturing conditions of chilling strip
As the manufacturing conditions of chilling strip, by the raw material 20g with each composition weighing shown in table 1 and table 2 at diameter
The water-cooled copper mold of about 40mm reduces pressure, Ar carries out arc-melting, makes the fusing mother metal of chilling strip.Chilling strip
Condition of making be, with single-roller method, this fusing mother metal to be placed in the quartz ampoule of diameter 15mm, tapping nozzle diameter is set to
1mm, with atmosphere pressure 61kPa, spraying pressure reduction 69kPa, the rotating speed 3000rpm of copper roller (diameter 300mm), copper roller and tapping nozzle
Gap 0.3mm tapping.Tapping temperature is set to the temperature after just the burning of each fusing mother metal.By thin for the chilling that so makes
Band, as test material, have rated following project.
The structure of chilling strip
As a rule, when measuring the X-ray diffractogram of non-crystalline material, can't see diffraction maximum, be the distinctive dizzy figure of amorphous.
It addition, be not completely in the case of amorphous, although it can be seen that diffraction maximum, but peak heights becomes compared with crystalline material
Low, and it can also be seen that dizzy figure.So utilizing following method to carry out non-crystalline evaluation.
As non-crystalline evaluation, utilize two-sided tape patch test material on a glass, utilize X-ray diffraction device
Obtain diffraction pattern.Now, glass will be attached to for test material in the mode making copper roller contact surface that mensuration face is chilling strip
On plate.X-ray source is Cu-K alpha ray, is determined with the scanning speed of 4 °/min.To can confirm that in this diffraction pattern
Dizzy figure be set to zero, by can't see completely being set to of dizzy figure ×, have rated amorphism.
The corrosion resistance (NaCl) of chilling strip
Utilize two-sided tape to attach for test material on a glass, carry out the brine spray examination of 5%NaCl-35 DEG C of-16h
Test, whole rust of looking unfamiliar is set to ×, is got rusty in local and be set to zero, evaluated.
Corrosion resistance (the HNO of chilling strip
3
)
Weigh the test material that supplies of 50mg, the 3at.%HNO of dropping 10ml3After aqueous solution, after at room temperature placing 1hr,
Analyze to 3%HNO3Co stripping quantity in aqueous solution.Co stripping quantity is set to zero less than 500ppm, by more than 500 and not enough
1000ppm is set to △, by being set to of more than 1000ppm ×.
The hardness of chilling strip
Chilling strip is longitudinally carried out resin embedding grinding, utilizes Vickers to measure.Mensuration load is 50g, with n
=10 are evaluated by meansigma methods.More than 1000HV is set to ◎, by 760～is set to zero less than 1000HV, by less than 760HV
It is set to △.
The saturation flux density of chilling strip
Utilize VSM device (vibration sample type magnetometer), be determined with the externally-applied magnetic field of 1200kA/m.For test material
The weight of material is about 15mg, and the test material that supplies of more than 0.3T and the saturation flux density less than 1.0T is set to zero, will
More than 1.0T is set to ◎.By being set to less than 0.3% ×.
Hereinafter, the one-tenth representing the present invention in table 1 and table 2 is grouped into, it addition, be expressed as its effect in table 3,4
The saturation flux density of fruit, amorphism, corrosion resistance, hardness.
[table 1]
Table 1
[table 2]
Table 2
Note) underscore represents outside condition of the present invention
[table 3]
Table 3
[table 4]
Table 4
First, the one-tenth shown in table 1 and table 2 is grouped into illustrates.No.1 shown in table 1～32 is example of the present invention, table 2
Shown No.33～41 is comparative example.
And, the record being grouped into for one-tenth, if as a example by the No.3 described in table 1 respectively arranges, then as (A)～(F)
The Ta that (A) of group element organizes is 8at.%, and the Cr that (B) organizes is 2at.%, and the Zr that (C) organizes is 4at.%, and the Al that (E) organizes is
1at.%, the B that (F) organizes are the content of 6at.%.Their total amount is 21at.%.(A) remainder that group～(F) organize is Co
And Fe, in an amount of from the 79at.% deducting 21at.% from 100.Additionally, the ratio of Co and Fe is Co: Fe=90: 10, if therefore
For at.%, then mean that the content that content is 0.79 × 90=71.1at.%, Fe of Co is 0.79 × 10=
7.9at.%.
Comparative example No.33, No.34 are owing to (A) group element is with the content of (B) group element and high, and therefore saturation flux is close
Spend low.No.35 is low due to the content of (A) group element, and therefore amorphism is not enough, and additionally hardness is the lowest.No.36 is due to (B) constituent element
The content of element is low, and therefore amorphism is not enough, and additionally corrosion resistance is the most not enough.The content magnetic high, saturated of (C) group element of No.37
Flux density is low.The content of (E) group element of No.38 is high and saturation flux density is low.The content of (F) group element of No.39 high and
Saturation flux density is low, it addition, corrosion resistance is the most abundant.No.40 is low due to Fe ratio, and therefore saturation flux density is filled not
Point.
No.41 is high due to Fe ratio, therefore corrosion resistance, particularly not enough to the corrosion resistance of NaCl.(D) group of No.42
The content of element is high, saturation flux density is low.On the other hand, it is known that example No.1 of the present invention～No.32 are owing to meeting the present invention
Condition, therefore amorphism, hardness, corrosion resistance and saturation flux density are excellent.
As it has been described above, according to the present invention it is possible to provide amorphism, hardness, corrosion resistance and saturation flux density excellence
Perpendicular magnetic recording non-retentive alloy and sputtering target material and employ the magnetic recording media of this alloy.
The manufacture of sputtering target material
Below, the manufacture method of sputtering target material is given.No.3, No.11, No.12, No.13, No.24 and table for table 1
Shown in No.35, No.38 of 27 kind one-tenth is grouped into, and weighs melt raw material, in the refractory material crucible of decompression Ar gas atmosphere
After carrying out induction heating melting, tap from the nozzle of the diameter 8mm of crucible bottom, utilize Ar gas to be atomized.With this gas
Body atomized powder is as raw material, in the tank of the SC that degassing loads external diameter 220mm, internal diameter 210mm, long 200mm.By degassing time
Final vacuum is set to about 1.3 × 10-2Pa.After above-mentioned powder filling base is heated to 1150 DEG C, load diameter 230mm's
In restricted type container, the pressurization of 500MPa is utilized to form.The body that is solidified into profit made with the aforedescribed process utilizes line
Cutting, lathe process, plane lapping be processed as diameter 180mm, thick 7mm discoid, make sputtering target material.
The manufacture of sputtered film
This one-tenth of 7 kinds is grouped into use sputtering target material and forms sputtered film on the glass substrate.X-ray diffractogram
No.3, No.11, No.12, No.13, No.24 are it can be seen that dizzy figure, and No.35, No.38 see crystal peak.It addition, with urgency
Cold strip has carried out corrosion resistance test (salt spraytest) in the same manner, as a result of which it is, No.3, No.11, No.12, No.13,
No.24 does not the most get rusty, it can be seen that get rusty in local in No.35, No.38.If to summary carried out above, then confirm to utilize
The result of chilling strip evaluation is equal trend with the evaluation of the sputtered film using sputtering target material film forming.
Claims (10)
1. a magnetic recording non-retentive alloy, is to comprise in terms of at.%:
One kind or two or more in the A group element selected from Ta, Nb and V of more than 0.5%；
One kind or two or more in the B group element selected from Cr, Mo and W of more than 0.5%；
0～5% the C group element selected from Ti, Zr and Hf in one kind or two or more；
0～30% the D group element selected from Ni and Mn in a kind or 2 kinds；
0～5% the E group element selected from Al and Cu in a kind or 2 kinds；
0～10% the F group element selected from Si, Ge, P, B and carbon in one kind or two or more；Remainder is by Co and Fe
And the magnetic recording non-retentive alloy that inevitably impurity is constituted, wherein,
The ratio of Fe:Co is 10:90～70:30, and the total amount of A group element, B group element and C group element is described alloy
12.6～30%.
Alloy the most according to claim 1, it comprises:
More than 0% and be less than 30% described D group element in a kind or 2 kinds；
More than 0% and be less than 5% described E group element in a kind or 2 kinds；
More than 0% and be less than 10% described F group element in one kind or two or more.
Alloy the most according to claim 1, its comprise 2～20% described A group element in one kind or two or more.
Alloy the most according to claim 1, its comprise 1～20% described B group element in one kind or two or more.
Alloy the most according to claim 1, its comprise 2～4% described C group element in one kind or two or more.
Alloy the most according to claim 1, its comprise more than 0% and be less than 10% described D group element in a kind or
2 kinds.
Alloy the most according to claim 1, its comprise 1～4% described E group element in a kind or 2 kinds.
Alloy the most according to claim 1, its comprise 1～8% described F group element in one kind or two or more.
9. a sputtering target material, it is made up of the alloy according to any one of claim 1～8.
10. a magnetic recording media, it possesses the soft ferromagnetic layer being made up of the alloy according to any one of claim 1～8.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2011030562A JP5698023B2 (en) | 2011-02-16 | 2011-02-16 | Soft magnetic alloy for magnetic recording, sputtering target material, and magnetic recording medium |
| JP2011-030562 | 2011-02-16 | ||
| PCT/JP2012/053164 WO2012111568A1 (en) | 2011-02-16 | 2012-02-10 | Soft magnetic alloy for magnetic recording, sputtering target material and magnetic recoding medium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103380458A CN103380458A (en) | 2013-10-30 |
| CN103380458B true CN103380458B (en) | 2016-11-30 |
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