CN106795620A - Magnetic material sputtering target - Google Patents
Magnetic material sputtering target Download PDFInfo
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- CN106795620A CN106795620A CN201580008580.1A CN201580008580A CN106795620A CN 106795620 A CN106795620 A CN 106795620A CN 201580008580 A CN201580008580 A CN 201580008580A CN 106795620 A CN106795620 A CN 106795620A
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- powder
- sputtering target
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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
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing Of Magnetic Record Carriers (AREA)
- Physical Vapour Deposition (AREA)
- Magnetic Record Carriers (AREA)
Abstract
A kind of sputtering target, it is with the metal matrix phase containing Fe and forms particle and disperse the sputtering target of the non-magnetic phase for existing, it is characterized in that, non-magnetic phase contains 0.1~40 mole of C of %, the X-ray diffraction of the sputtering target it is unimodal among the integral breadth of intensity highest diffraction maximum be less than 0.8.The present invention provides a kind of nonmagnetic substance particle dispersion-type sputtering target, and the generation of primary powder particles when it passes through to suppress sputtering is so as to reduce burn-in time, and the electric discharge that can be stablized in sputtering.
Description
Technical field
The present invention relates to be used for the magnetic film of magnetic recording media, the hard disk especially with perpendicular magnetic recording
The ferromagnetic material sputtering target of the film forming of magnetic recording layer, and it is related to primary powder particles few, electric discharge that is being stablized in sputtering
Nonmagnetic substance particle dispersion-type sputtering target.
Background technology
In the magnetic recording field with hard disk drive as representative, as the material of the thin magnetic film in magnetic recording media, make
With the material that Co, Fe or the Ni as ferromagnetism metal are matrix.For example, in the magnetic using the hard disk of return to zero in face
The Co-Cr bases or Co-Cr-Pt base strong magnetic alloys using Co as main component are used in property film.
In addition, using in recent years practical perpendicular magnetic recording hard disk thin magnetic film in, use more comprising with
Co is used as the Co-Cr-Pt bases strong magnetic alloy of main component and the composite of non-magnetic inorganic thing particle.And, from production
From the viewpoint of rate is high, above-mentioned thin magnetic film utilizes DC magnetron sputterings frequently by by the sputtering target using above-mentioned material as composition
Device is sputtered to make.
On the other hand, the packing density of hard disk rapidly increases year by year, it is believed that in the future from 600 current gigabits/flat
The surface density of square inch reaches 1,000,000,000,000 bits/square inch.When packing density reaches 1,000,000,000,000 bits/square inch, record ratio
The size of special (bit) is less than 10nm, in such a case, it is possible to expect that the superparamagnetic caused by thermal fluctuation turns into problem,
And it is anticipated that the material of the magnetic recording media for currently using, such as improved by adding Pt in Co-Cr based alloys
The material of crystal magnetic anisotropy is insufficient.Because：Ferromagnetism is shown with the dimensionally stable of below 10nm
Particle need have crystal magnetic anisotropy higher.
In view of above-mentioned reason, with L10The FePt phases of structure are attracted attention as super high-density recording medium with material.Tool
There is L10The crystal magnetic anisotropy of the FePt phases of structure is high, and corrosion resistance, oxidation resistant, therefore, it is expected for fitting
It is the material of magnetic recording media application to cooperate.Also, when using FePt phases as super high-density recording medium material, it is desirable to
The FePt magnetic particles of ordering of sening as an envoy to are developed with the state of Magnetic isolation high density as far as possible and as one man scattered technology is orientated.
Due to situation as described above, it is proposed that will make with L10The FePt magnetic particles of structure utilize oxide, carbon
Etc. (C) thin magnetic film of the granular texture of nonmagnetic substance isolation is used as using the hard disk of future generation of HAMR mode
Magnetic recording media.The granular texture thin magnetic film forms the magnetic particle magnetic because namagnetic substance is present between them each other
The structure of insulation.As the magnetic recording media with granular texture thin magnetic film and relative known document, example can be enumerated
Such as patent document 1.
As above-mentioned containing with L10The granular texture thin magnetic film of the FePt phases of structure, is contained in terms of volume ratio
10%~50% carbon (C) is as the thin magnetic film of namagnetic substance especially because its magnetic characteristic is high and attracts attention.It is known this
The granular texture thin magnetic film of sample is sputtered simultaneously by using the single element target of Fe targets, Pt targets, C targets, or uses Fe-Pt
Alloys target, C targets are sputtered to make simultaneously.However, in order that sputtered with these sputtering targets, it is necessary to expensive same simultaneously
When sputter equipment.
Therefore, in batch production, entered using the one-piece type sinter sputtering target comprising Fe based alloys and nonmagnetic substance
The making of row thin magnetic film.But, when smart (machinery) is processed, the non-magnetic phase exposed on surface is subject to lack such target sometimes
Damage, squeeze crack (む れ) equivalent damage, there is accident in sputtering and come off or cause paradoxical discharge in it, so that powder (is attached to
Foreign matter on substrate) the increased problem of generation.
It is in the past to use the scheme for reducing surface roughness in order to solve such problem more.For example, patent document 2 is instructed
It is a kind of to enter to be about to the surface roughness of sputtering target and be adjusted to Ra≤1.0 μm etc., so as to suppress the generation of dross and suppress powder
Generation technology.However, sputtering target disclosed herein is due in the absence of non-magnetic particles such as oxides, thus target surface machine
Tool processing is easy, is easier to realize the inhibition of powder, but exist cannot be used for it is non magnetic as the present invention
The problem of the sputtering target of particle fine dispersion.
In addition, as other schemes, for the sputtering target for not containing nonmagnetic substance, in order to reduce primary powder particles
(shortening burn-in time), also carries out removing processing by the chemical method of etching etc. rather than by physical methods such as machinings
Strain.However, in the case of containing carbon (C), the magnetic material target of oxide in the metals such as Fe, Pt, it is impossible to carry out good
Etching, it is impossible to carry out the improvement of the surface roughness same with the target comprising single element.
In addition, Patent Document 3 discloses it is a kind of realized by removing the surface deformation later of sputtering target shorten sputtering when
Burn-in time technology.The surface treatment method by target surface is contacted with visco-elastic abrasive medium (VEAM) and to target table
Face carries out extrusion honing polishing.However, such surface treatment method is have for the metal material in the absence of non-magnetic particle
Effect, and in the case of the target for being applied to have non-magnetic particle, there is a problem of that these non-magnetic particles come off.
Prior art literature
Patent document
Patent document 1：Japanese Unexamined Patent Publication 2004-152471 publications
Patent document 2：Japanese Unexamined Patent Publication 11-1766 publications
Patent document 3：Japanese Unexamined Patent Application Publication 2010-516900 publications
The content of the invention
Invent problem to be solved
As described above, in the case of containing magnetic material targets of the nonmagnetic substance such as metal material and carbon (C) such as Fe, exposing
Non-magnetic phase in target surface is subject to defect, squeeze crack equivalent damage due to machining, and powder is produced when there is sputtering increases this
The problem of sample.Even if in addition, can solve the problem that the machining turn into reason non-magnetic phase defect, the problem of squeeze crack, with table
Face is machined associated remaining processing strain and is present in target, and this also turns into powder Producing reason.Especially since this is residual
The assurance of remaining processing strain is simultaneously insufficient, thus precision to method of surface finish and processing impacts, and is not implemented from basic
Upper solution powder is produced.
The means used to solve the problem
It is above-mentioned in order to solve the problems, such as, present inventor has performed further investigation, as a result find, by reducing during machining
Non-magnetic phase defect, squeeze crack, and the remaining processing strain of sputtering target is reduced, with the integral breadth at the peak of X-ray diffraction
The degree of remnants processing strains is identified, it is possible thereby to provide nonmagnetic substance particle dispersion-type sputtering target, the sputtering target can
The generation of primary powder particles when suppressing sputtering is so as to significantly shorten burn-in time, and the electric discharge that can be stablized in sputtering.
Based on the discovery that, the present invention is provided：
1) a kind of sputtering target, it is with the metal matrix phase containing Fe and forms particle and disperse the non magnetic of presence
The sputtering target of phase, it is characterised in that contain 0.1~40 mole of C of %, the X-ray diffraction of the sputtering target as non-magnetic phase
It is unimodal among intensity highest diffraction maximum integral breadth be less than 0.8.
2) sputtering target as described in 1), it is characterised in that in metal matrix phase, Pt is 33 moles of more than % and 56 mole of %
Below, remainder is Fe and inevitable impurity.
1) or 2) 3) sputtering target as described in, it is characterised in that
As non-magnetic phase contain 5~25 moles of % selected from SiO2、TiO2、Ti2O3、Cr2O3、Ta2O5、Ti5O9、B2O3、
CoO、Co3O4One or more of oxide.
4) as 1)~3) any one of sputtering target, it is characterised in that
Metal matrix containing 0.1 mole of %~10 mole % selected from Ag, Cu, B, Ti, V, Mn, Zr, Nb, Ru, Mo,
One or more of Ta, W element.
Invention effect
The present invention can provide a kind of nonmagnetic substance particle dispersion-type sputtering target, and it can suppress initial powder during sputtering
The generation of grain is so as to significantly shorten pre-burning (burn-in) time, and the electric discharge that can be stablized when being sputtered.In addition,
Thus target lifetime extension, can be with low cost manufacture magnetic film.Also having can significantly improve by sputtering the film for being formed
The effect of quality.
Specific embodiment
Constituting the composition of sputtering target of the invention has the metal matrix phase containing Fe and forms particle and disperse what is existed
Non-magnetic phase.And, it is characterised in that X-ray diffraction it is unimodal among intensity highest diffraction maximum integral breadth for 0.8 with
Under.This turns into the index that remaining processing strain is reduced.Thereby, it is possible to reduce remaining processing strain, therefore result from remaining processing
The generation of the primary powder particles of strain is few, and burn-in time can be greatly decreased.
Integrated value evaluation on X-ray diffraction peak, according to JCPDS cards：03-065-4899, it is known that the X-ray of α-Fe
In 2 θ=44.66 ° it was observed that belonging to the peak in (111) face, the peak for belonging to (200) face being observed at 65.01 ° in diffraction maximum.
In addition, according to JCPDS cards：01-074-4586, it is known that Fe3Observed at 42.50 ° in the X-ray diffraction peak of Pt and belonged to
(202) peak in face, the peak for belonging to (220) face is observed at 44.70 °.However, in the case of the target comprising Fe-Pt alloys,
Even if observing X-ray diffraction peak near 44.7 °, the peak that judgement is derived from belonging to α-Fe (111) face is also difficult to sometimes, also
It is derived from belonging to Fe3The peak in Pt (220) face, or the totalling for being derived from them.
Therefore, the present invention in, as the X-ray diffraction peak evaluated for integral breadth, be set as never with other peaks
The unimodal middle selection of the possibility of overlap.In addition, wherein, in order that the influence of evaluated error is minimum, selecting unimodal middle intensity most
Peak high.The size for processing strain influences peak position and peak width in X-ray diffraction.In the state that the deviation of spacing of lattice is constant
Under by cause its average value be decreased or increased in the way of produce strain in the case of, do not influence peak width, only peak position is to high angle
Side or low angle side offset.However, when assigning processing strain, the actually deviation increase of spacing of lattice, therefore peak width increases sometimes
Greatly, while peak position also offsets to a certain extent.Therefore, the sizableness of peak width is quantitatively compared in the size for comparing strain.
Also, the index of the width as peak, to can be used and influence few integral breadth by what condition determination was caused.Herein, integral breadth
Refer to the integral area at peak divided by value obtained from peak intensity.
In the present invention, as metal matrix phase, Pt is 33 moles of more than % and 56 mole of below %, remainder is Fe
It is representational composition with the sputtering target of inevitable impurity, the present application includes these sputtering targets.These sputtering targets are
Magnetic film in magnetic recording media, especially with perpendicular magnetic recording hard disk magnetic recording layer film forming in use
Ferromagnetic material sputtering target.
In addition, as non-magnetic phase, at least containing 0.1~40 mole of carbon of % (C).If the C particles in sputtering target composition
Content be less than 0.1 mole of %, then the magnetic interaction between carbon can not make magnetic particle in the thin magnetic film is fully insulated, therefore
Sometimes cannot get good magnetic characteristic, if in addition, being more than 40 moles of %, C particle buildups, produce thick in target tissue sometimes
C phases, so as to increase the generation of powder.
In addition, as non-magnetic phase, in addition to the carbon (C) being described above, can also enumerate selected from SiO2、TiO2、
Ti2O3、Cr2O3、Ta2O5、Ti5O9、B2O3、CoO、Co3O4One or more of oxide.The target of the present application contains 5~25
These oxides of mole %.It should be noted that in embodiment described later, the example of their part is illustrate only,
But it is respectively provided with function substantially of equal value as non-magnetic phase.
Additionally, in sputtering target of the invention, as metal matrix phase, 0.1 mole of more than % and 10 mole of % can be contained
It is following selected from one or more of Ag, Cu, B, Ti, V, Mn, Zr, Nb, Ru, Mo, Ta, W element.These are to improve conduct
The characteristic of magnetic recording media and the element that is added as needed on.Mixing ratio can be set as above range, can keep making
It is the characteristic of effective magnetic recording media.
Sputtering target of the invention can be made by powder sintering.
First, the powder of the metallic element of each metallic element is prepared.These powder preferably use particle diameter for more than 0.5 μm and
Less than 10 μm of powder.When the particle diameter of powder is too small, there is oxidation and be promoted so that oxygen concentration in sputtering target rises etc. asks
Topic, therefore preferably more than 0.5 μm.On the other hand, if the particle diameter of powder is big, it is difficult to make C particles fine dispersion in the alloy,
Therefore less than 10 μm of powder is preferably used.
Further, it is possible to use the alloy powder (such as Fe-Pt powder) of these metals replaces the powder of each metallic element.Especially
It is, for the alloy powder comprising Pt, although depending on its composition, but is have for reducing the oxygen amount in material powder
Effect.In the case of using alloy powder, it is also preferred that using the powder that particle diameter is more than 0.5 μm and less than 10 μm.
Then, these metal dust is weighed according to desired composition, is used the known method such as ball mill
Crushed and mixed.In the case where non-magnetic particle is added, mixed with metal dust in the stage.
As the powder of non-magnetic particle, prepare C powder and oxide powder, the powder of non-magnetic particle preferably uses grain
Footpath is the powder of more than 0.5 μm and less than 10 μm.When the particle diameter of powder is too small, easily aggregation, therefore preferably more than 0.5 μm,
On the other hand, if particle diameter is big, the generating source as powder, therefore preferably use less than 10 μm of powder.
Then, after above-mentioned powder is weighed according to desired composition, using grater by above-mentioned raw materials powder
Crush and mix.Herein, as mixing arrangement, it is possible to use ball mill, mortar etc., the mixing of the strengths such as ball mill is preferably used
Method.If in addition, considering the problem of the oxidation in mixing, being mixed preferably in inert gas atmosphere or in vacuum.
So obtained mixed-powder is formed and sintered using hot-press arrangement, so as to be made sintered body.Shaping and
Sintering is not limited to hot pressing, it is also possible to use discharge plasma sintering process, HIP sintering method.Though keeping temperature during sintering
So depending on the composition of target, but in most cases it is set as 1100 DEG C~1400 DEG C of temperature range.
Afterwards, taken out from hot-press arrangement, high temperature insostatic pressing (HIP) processing is carried out to sintered body.This is for improving the close of sintered body
Spend effective means.Although keeping temperature when high temperature insostatic pressing (HIP) is processed also depends on the composition of target, but in most cases sets
It is 1100 DEG C~1400 DEG C of temperature range.In addition, moulding pressure is set as more than 100MPa.Then, will be such using lathe
The sintered body for obtaining is processed into desired shape.
It is important that remaining processing strain is removed in the present invention, and Plane of rotation grinding is carried out after lathe process, it
Carry out afterwards using the attrition process (finishing) of abrasive particle.The evaluation processed based on these is by observing the peak of XRD (X-ray diffraction)
Come carry out.Then so that XRD it is unimodal among the integral breadth at the most strong peak of intensity be less than 0.8.
The integral breadth at the peak (referring to crystal face) by X-ray diffraction measure of above-mentioned target reflects included in the crystal face interior
Portion is strained, and it is produced due to the processing strain carried out during the machinings such as plastic working, target cutting when target is manufactured.
In this case, integral breadth is bigger (peak is wider), it is meant that overstrain is big.
Its final evaluation depends on the species and Surface Machining of raw material, thus a certain degree of experiment is repeated, and makes
Obtaining can reach target.If surface processing technique once it is determined that, can consistently obtain cause XRD it is unimodal among intensity most
The integral breadth at strong peak is less than 0.8 condition.These can be described as this area skill if clearly the present application is held
The condition that art personnel are readily obtained.So carry out, the sputtering target of non-magnetic particle fine dispersion can be manufactured.
Embodiment
Hereinafter, illustrated based on embodiment and comparative example.It should be noted that the present embodiment is only one, this hair
It is bright to be not limited to the example.That is, the present invention is limited only by the following claims, also including embodiment contained in the present invention beyond it is various
Deformation.
(embodiment 1)
As material powder, prepare Fe powder, the Pt powder of 3 μm of average grain diameter, 1 μm of the average grain diameter of 3 μm of average grain diameter
TiO2The C powder of powder, 1 μm of average grain diameter.C powder uses commercially available amorphous carbon.For these powder, according to the group of target
As Fe-40Pt-9TiO2- 10C (mole %) weighs Fe powder, Pt powder, the TiO of total weight 2600g2Powder, C powder.
Then, the powder of weighing is enclosed the ball grinder of 10 liters of capacity together with the titanium dioxide ball as crushing medium
In, rotate 4 hours and mixed and crushed.Then, the mixed-powder taken out from ball mill is filled into carbon molding jig
And carry out hot pressing.When the condition of hot pressing is set as vacuum atmosphere, 300 DEG C/h of programming rate, 1200 DEG C of keeping temperature, holding
Between 2 hours, since heat up start up to keep end pressurizeed with 30MPa.Holding terminate after in chamber former state natural cooling.
Then, implement high temperature insostatic pressing (HIP) for the sintered body taken out from the mould of hot press to process.High temperature insostatic pressing (HIP) processing
Condition is set as 300 DEG C/h of programming rate, 1100 DEG C of keeping temperature, 2 hours retention times, is slowly carried when heating up
The gas pressure of Ar gases high, is pressurizeed during being maintained at 1100 DEG C with 150MPa.Holding is former in stove after terminating
Sample natural cooling.Lathe process is carried out to such sintered body for making, Plane of rotation grinding is carried out afterwards, then carry out profit
With the attrition process (finishing) of abrasive particle, so as to obtain the discoid target of diameter 180mm, thickness 5mm.Plane of rotation is ground
The processing capacity of processing is set as 50 μm, and the processing capacity of attrition process (finishing) is set as 3 μm.
In order to speculate the overstrain in the target remained on surface, carried out XRD (X-ray diffraction) measure, it is as a result unimodal in
The integral breadth of the diffraction maximum near 2 θ=41 ° of maximum intensity is 0.6, in the range of the present application.Need explanation
It is to be set as tube voltage 40kV, tube current 30mA, sweep as device, condition determination is determined using company system UltimaIV of science
Retouch 0.005 ° of °/minute of speed 1, step-length.
Then, the target is arranged in magnetic control sputtering device (Canon ANELVA C-3010 sputtering systems), and is carried out
Sputtering.The condition of sputtering is set as input power 1kW, Ar gas pressure 1.7Pa, straight at 4 inches after implementing the pre-sputtering of 2kWh
The film forming of 20 seconds is carried out with 1kW on the silicon substrate in footpath.
Then, the number of the powder with powder counter to adhering on substrate is measured.As a result, 0.4kWh is being carried out
Sputtering moment, powder number reduced to background level (5) below.That is, will can stablize needed for the characteristic of sputtering target when
Between (burn-in time) foreshorten to 0.4kWh.It should be noted that due to production can not be started during pre-burning is carried out, therefore in advance
The burning time is more short more preferred, is desired for below 1.0kWh.
(embodiment 2)
By method similarly to Example 1, composition has been made for Fe-40Pt-9TiO2The sintering of -10C (mole %)
Body.Lathe process is carried out to the sintered body, flat surface grinding processing is carried out afterwards, so as to obtain diameter 180mm, thickness 5mm
Discoid target.Finishing is implemented also by flat surface grinding, is implemented under conditions of cutting output is set as into infinite approach zero
Finishing.The processing capacity of flat surface grinding processing is set as 50 μm, wherein finishing is set as 1 μm.In order to speculate on the target surface
The overstrain of residual, has carried out XRD (X-ray diffraction) measure, as a result unimodal middle intensity under the same conditions as example 1
The integral breadth of the diffraction maximum near 2 maximum θ=41 ° is 0.8, in the range of the present application.
Then, sputtered under conditions of similarly to Example 1 using the target, with powder counter to adhering on substrate
The number of powder be measured.As a result, in the sputtering for carrying out 0.8kWh, powder number is reduced to background level (5
It is individual) below.That is, the time (burn-in time) needed for can stablizing the characteristic of sputtering target foreshortens to 0.8kWh.Need explanation
It is that due to that can not start production during pre-burning is carried out, therefore burn-in time is more short more preferred, is desired for below 1.0kWh.
(embodiment 3)
As material powder, prepare Fe powder, the Pt powder of 3 μm of average grain diameter, 5 μm of the average grain diameter of 3 μm of average grain diameter
B2O3The C powder of powder, 2 μm of average grain diameter.It is Fe-40Pt-5B according to the composition of target for these powder2O3- 14C (rubs
You are %) weigh Fe powder, Pt powder, the B for adding up to weight 2500g2O3Powder, C powder.
Then, the powder of weighing is enclosed in the ball grinder of 10 liters of capacity together with the steel ball as crushing medium, rotation 4
Hour and mixed and crushed.Then, the mixed-powder taken out from ball mill is filled into carbon molding jig and carries out heat
Pressure.The condition of hot pressing is set as vacuum atmosphere, 300 DEG C/h of programming rate, 1000 DEG C of keeping temperature, 2 hours retention times,
Pressurizeed with 30MPa up to holding end since heating up.Holding terminate after in chamber former state natural cooling.
Then, high temperature insostatic pressing (HIP) processing is implemented to the sintered body taken out from the mould of hot press.The bar of high temperature insostatic pressing (HIP) processing
Part is set as 300 DEG C/h of programming rate, 1100 DEG C of keeping temperature, 2 hours retention times, is slowly carried since heating up
The gas pressure of Ar gases high, is pressurizeed during being maintained at 1100 DEG C with 150MPa.Holding is former in stove after terminating
Sample natural cooling.Lathe process is carried out to such sintered body for making, Plane of rotation grinding is carried out afterwards, then carry out profit
With the attrition process (finishing) of abrasive particle, so as to obtain the discoid target of diameter 180mm, thickness 5mm.Plane of rotation is ground
The processing capacity of processing is set as 50 μm, and the processing capacity of attrition process (finishing) is set as 3 μm.
In order to speculate the overstrain in the target remained on surface, XRD has been carried out under the same conditions as example 1, and (X is penetrated
Line diffraction) determine, the integral breadth of the diffraction maximum near 2 θ=41 ° of as a result unimodal middle maximum intensity is 0.7, in the application hair
In bright scope.Then, the target is arranged in magnetic control sputtering device (Canon ANELVA C-3010 sputtering systems), is gone forward side by side
Row sputtering.The condition of sputtering is set as input power 1kW, Ar gas pressure 1.7Pa, after implementing the pre-sputtering of 2kWh, at 4 inches
The film forming of 20 seconds is carried out with 1kW on the silicon substrate of diameter.
Then, the number of the powder with powder counter to adhering on substrate is measured.As a result, 0.4kWh is being carried out
Sputtering moment, powder number reduced to background level (5) below.That is, will can stablize needed for the characteristic of sputtering target when
Between (burn-in time) foreshorten to 0.6kWh.It should be noted that production can not be started during pre-burning is carried out, therefore during pre-burning
Between it is more short more preferred, be desired for below 1.0kWh.
(embodiment 4)
By method similarly to Example 3, composition has been made for Fe-40Pt-5B2O3The sintered body of -14C (mole %).
Lathe process is carried out to the sintered body, flat surface grinding processing is carried out afterwards, so as to obtain the disk of diameter 180mm, thickness 5mm
The target of shape.Finishing is implemented also by flat surface grinding, and finishing is implemented under conditions of cutting output is set as into infinite approach zero
Work.The processing capacity of flat surface grinding processing is set as 50 μm, wherein finishing is set as 1 μm.In order to speculate in the target remained on surface
Overstrain, carried out under the same conditions as example 1 XRD (X-ray diffraction) measure, as a result unimodal middle maximum intensity
2 θ=41 ° near diffraction maximum integral breadth be 0.8, in the range of the present application.
Then, sputtered under conditions of similarly to Example 1 using the target, with powder counter to adhering on substrate
The number of powder be measured.As a result, in the sputtering for carrying out 0.9kWh, powder number is reduced to background level (5
It is individual) below.That is, the time (burn-in time) needed for can stablizing the characteristic of sputtering target foreshortens to 0.9kWh.Need explanation
It is that can not start production during pre-burning is carried out, therefore burn-in time is more short more preferred, is desired for below 1.0kWh.
(comparative example 1)
Carry out similarly to Example 1, made composition for Fe-40Pt-9TiO2The target of -10C (mole %).But,
When being machined to sintered body, only with lathe process.In order to speculate the overstrain in the target remained on surface, with reality
Apply and carried out under the conditions of the identical of example 1 XRD (X-ray diffraction) measure, spreading out near 2 θ=50 ° of as a result unimodal middle maximum intensity
It is 1.2 to penetrate the integral breadth at peak, beyond the scope of the present application.Entered under conditions of similarly to Example 1 using the target
Sputtering is gone, as a result in the sputtering for carrying out 1.5kWh, powder number is reduced to background level (5) below.That is pre-burning
Time is 1.5kWh, more long than embodiment 1.
(comparative example 2)
By method similarly to Example 3, composition has been made for Fe-40Pt-5B2O3The sintered body of -14C (mole %).
But, when being machined to sintered body, only with lathe process.In order to speculate that the remnants in the target remained on surface should
Become, carried out XRD (X-ray diffraction) measure under the same conditions as example 1,2 θ of as a result unimodal middle maximum intensity=
The integral breadth of the diffraction maximum near 50 ° is 1.6, beyond the scope of the present application.Using the target similarly to Example 1
Under conditions of sputtered, as a result in the sputtering for carrying out 2.2kWh, powder number reduce to background level (5) with
Under.That is, burn-in time is 2.2kWh, more long than embodiment 3.
[table 1]
Industrial applicability
The present invention provides a kind of nonmagnetic substance particle dispersion-type sputtering target, primary powder particles when it can suppress to sputter
Produce so as to burn-in time is greatly decreased, and the electric discharge that can be stablized in sputtering.Target lifetime extend, can with it is low into
This manufacture magnetic film.Furthermore it is possible to significantly improve the quality by sputtering the film for being formed.As the magnetic in magnetic recording media
The ferromagnetic material sputtering target used in gonosome film, the especially film forming of hard disk drive recording layer is useful.
Claims (4)
1. a kind of sputtering target, it is with the metal matrix phase containing Fe and forms particle and disperse the non-magnetic phase for existing
Sputtering target, it is characterised in that non-magnetic phase contains 0.1~40 mole of C of %, the X-ray diffraction of the sputtering target it is unimodal it
The integral breadth of middle intensity highest diffraction maximum is less than 0.8.
2. sputtering target as claimed in claim 1, it is characterised in that in metal matrix phase, Pt is that 33 moles of more than % and 56 are rubbed
That below %, remainder are Fe and inevitable impurity.
3. sputtering target as claimed in claim 1 or 2, it is characterised in that
Non-magnetic phase contain 5~25 moles of % selected from SiO2、TiO2、Ti2O3、Cr2O3、Ta2O5、Ti5O9、B2O3、CoO、Co3O4
One or more of oxide.
4. the sputtering target as any one of claims 1 to 3, it is characterised in that
Metal matrix containing 0.1 mole of %~10 mole % selected from Ag, Cu, B, Ti, V, Mn, Zr, Nb, Ru, Mo, Ta, W
More than one elements.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210309573.7A CN114807874A (en) | 2014-03-18 | 2015-03-13 | Magnetic material sputtering target |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2014055092 | 2014-03-18 | ||
| JP2014-055092 | 2014-03-18 | ||
| PCT/JP2015/057428 WO2015141571A1 (en) | 2014-03-18 | 2015-03-13 | Magnetic sputtering target |
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| CN202210309573.7A Division CN114807874A (en) | 2014-03-18 | 2015-03-13 | Magnetic material sputtering target |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202210309573.7A Pending CN114807874A (en) | 2014-03-18 | 2015-03-13 | Magnetic material sputtering target |
| CN201580008580.1A Pending CN106795620A (en) | 2014-03-18 | 2015-03-13 | Magnetic material sputtering target |
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| CN202210309573.7A Pending CN114807874A (en) | 2014-03-18 | 2015-03-13 | Magnetic material sputtering target |
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|---|---|
| JP (1) | JP6030271B2 (en) |
| CN (2) | CN114807874A (en) |
| MY (1) | MY173140A (en) |
| SG (1) | SG11201604730PA (en) |
| WO (1) | WO2015141571A1 (en) |
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| US20080202916A1 (en) * | 2007-02-22 | 2008-08-28 | Heraeus Incorporated | Controlling magnetic leakage flux in sputtering targets containing magnetic and non-magnetic elements |
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| JP2000169960A (en) * | 1998-12-04 | 2000-06-20 | Japan Energy Corp | Sputtering target for forming optical disk recording film |
| JP2009191359A (en) * | 2008-01-15 | 2009-08-27 | Hitachi Metals Ltd | Fe-Co-Zr BASED ALLOY TARGET MATERIAL |
| JP4673448B2 (en) * | 2009-03-27 | 2011-04-20 | Ｊｘ日鉱日石金属株式会社 | Non-magnetic particle dispersed ferromagnetic sputtering target |
| MY167825A (en) * | 2012-06-18 | 2018-09-26 | Jx Nippon Mining & Metals Corp | Sputtering target for magnetic recording film |
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2015
- 2015-03-13 CN CN202210309573.7A patent/CN114807874A/en active Pending
- 2015-03-13 JP JP2016508691A patent/JP6030271B2/en active Active
- 2015-03-13 WO PCT/JP2015/057428 patent/WO2015141571A1/en active Application Filing
- 2015-03-13 SG SG11201604730PA patent/SG11201604730PA/en unknown
- 2015-03-13 MY MYPI2016702439A patent/MY173140A/en unknown
- 2015-03-13 CN CN201580008580.1A patent/CN106795620A/en active Pending
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| CN101278071A (en) * | 2005-10-04 | 2008-10-01 | 日矿金属株式会社 | Sputtering target |
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Also Published As
| Publication number | Publication date |
|---|---|
| JP6030271B2 (en) | 2016-11-24 |
| JPWO2015141571A1 (en) | 2017-04-06 |
| MY173140A (en) | 2019-12-31 |
| WO2015141571A1 (en) | 2015-09-24 |
| CN114807874A (en) | 2022-07-29 |
| SG11201604730PA (en) | 2016-08-30 |
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