CN104032274A - CoCrPt series alloy sputtering target and film and preparation method thereof - Google Patents
CoCrPt series alloy sputtering target and film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a CoCrPt series alloy sputtering target and film and a preparation method thereof. The CoCrPt series alloy sputtering target comprises an element B, wherein the content of the element B is 0-20 atomic percent; the alloy target comprises a Co-enriched phase and a B-enriched phase; the B-enriched phase is uniformly distributed in the Co-enriched phase; the average grain size of the Co-enriched phase is 20-50mu m; and the average grain size of the B-enriched phase is 0-20mu m. The method for preparing the CoCrPt series alloy sputtering target comprises the following steps: (1) performing vacuum melting; (2) performing hot isostatic pressure; (3) performing thermal machining; and (4) performing cold machining. The invention also discloses a magnetic recording medium prepared by using the CoCrPt series alloy sputtering target. The magnetic recording medium comprises a substrate layer, an adhesive layer, a soft magnetic layer, an intermediate layer and a magnetic recording layer, wherein the coercive force of the magnetic recording medium is 3000-5000Oe; and the squareness is 0.80-0.95. The CoCrPt series alloy sputtering target is uniform in chemical components and small in deviated nominal composition, and the technical problems in a conventional preparation process that rolling cracking is caused, the yield is low, the mount of deviated nominal composition of the chemical components of the alloy target is large, the content of harmful impurities is extremely high are solved.
Description
Technical field
The invention belongs to containing Pt magnetic recording sputtering target material and magnetic recording media field, be specifically related to a kind of CoCrPt based alloy sputtering target material, film and preparation method thereof.
Background technology
1970, the material that Japan professor's rock rugged pretty is used while proposing perpendicular magnetic recording medium was CoCr alloy, originally people's research just collect in CoCrX alloy, wherein X material is generally elected Ta, Pt, Nb, B etc. as.Pt can strengthen the magnetocrystalline anisotropy of CoCr material; Cr is than be easier to separate out the grain boundary that forms rich Cr from crystal grain, thereby reduce intercrystalline friendship, changes Said and closes interaction; Add Ta and be conducive to separating out of Cr; B more easily separates out than Cr from crystal grain, thereby effectively reduces intercrystalline coupling.Therefore, CoCrPtB alloy sputtering target is used as magnetic recording layer or the coupling layer in hard disk widely.
But due to the interpolation of B element, make CoCrPt that original fragility is larger be associated golden fragility larger, room temperature unit elongation is less than 2%, therefore can only prepare such alloy sputtering target by hot worked mode.Patent documentation 1 (US7927434) discloses a kind of CoCrPtB alloy sputtering target and preparation method thereof, the method is prepared ingot blank by vacuum induction melting method, subsequently at 1100 ℃ of these ingot blanks of hot rolling, require its heat distortion amount between 15～40%, obtained the alloy target material of coercive force between 3282～3293Oe, and its grain-size is below 200 microns.The inventor repeats experiment to it and finds: (1) is used merely Co, Cr, and Pt, tetra-kinds of materials of B are prepared burden and are carried out induction melting by stoichiometric ratio, and because B easily volatilizees, the chemical composition of final ingot blank can depart from nominal formulated component; (2) can there is the founding defects such as pore unavoidably in the inside ingot that prepared by vacuum induction melting, due to the fragility of CoCrPtB alloy itself, even at the course of hot rolling of 1100 ℃, defect also can be expanded, form crackle, finally cause ingot blank brisement, thereby reduced greatly the yield rate of product.
Patent documentation 2 (US6797137) discloses a kind of CoCrPtB alloy sputtering target and preparation method thereof, mainly by using powder metallurgy method to prepare alloy target, the mechanical properties such as the unit elongation of the alloy target material of preparation and fracture characteristics all make moderate progress, but because powder metallurgic method need to be by operations such as powder process, ball millings, finally by mode compression mouldings such as vacuum hotpressing or hot isostatic pressings.Therefore compare with smelting process and have following defect: (1) chemical composition homogeneity is poor; (2) target gas content is higher, and density is prepared target lower than smelting process; (3) for uniform ingredients, to carry out long ball milling combination treatment, easily introduce impurity.Above-mentioned shortcoming finally causes film composition lack of homogeneity, and film uniformity is poor, and film easily produces the ill effects such as defect, finally affects the magnetism characteristic of film.
Problem based on above existence, the inventor has proposed a kind of Chemical Composition evenly and has departed from CoCrPtB alloy sputtering target that nominal composition is less, grain-size is tiny evenly, foreign matter content is low and preparation method thereof, the method not only guarantees that the Chemical Composition of the said products is even, foreign matter content is low, but also can improve finished product rate, a kind of magnetic recording media of preparation of target materials thus is also provided simultaneously, the magnetic recording layer surface particles of this magnetic recording media is tiny evenly, coercive force is high, and squareness is good.
Summary of the invention
The object of the present invention is to provide a kind of CoCrPt based alloy sputtering target material and film and preparation method thereof, described sputtering target, detrimental impurity constituent content is low, and grain-size is tiny evenly, and Chemical Composition is evenly and to depart from nominal composition less.
Another object of the present invention is to provide a kind of thin film magnetic recording medium that uses above-mentioned sputtering target material to prepare, tiny even, the non magnetic crystal boundary of this magnetic recording media crystal grain is obvious, and magnetic performance is good.
The first object of the present invention is to realize like this, described CoCrPt based alloy sputtering target material also comprises B element, the content of described B element is 0～20 atomic percent, described alloy target material comprises rich Co phase and rich B two thing phases mutually, wherein rich B be evenly distributed in mutually rich Co mutually in, the average grain size of described rich Co phase is at 20～50 μ m, and the average grain size of rich B phase is at 0～20 μ m.
Described alloy target material is Co11.5Cr22Pt10B or Co13Cr16Pt10B.
Described alloy target material also comprises Si, Ti, Ta, Y, one or more in the elements such as Zr.
The actual content of described each element of alloy target material and the deviation <0.5at% of nominal content.
The C content <50ppm of described alloy target material, O content <50ppm, S content <10ppm, N content <10ppm.
The coercive force of described alloy sputtering target is at 3500～4500Oe, and described alloy target material thickness is when the thickness of 4～9mm, and its magnetic susceptibility is between 50%～80%.
A method of preparing described CoCrPt based alloy sputtering target material, comprising:
(1) vacuum melting: material is prepared burden by stoichiometric ratio, described vacuum melting is intermediate frequency vacuum induction melting, institute's use crucible for aluminum oxide or zirconium white crucible, pouring temperature be 1500～1650 ℃, before casting, melt includes the process of setting of at least 1 time in crucible;
(2) hot isostatic pressing: described ingot casting need pass through hip treatment, 800～1100 ℃ of temperature, 4N high-purity Ar atmosphere, pressure is 150～200MPa, soaking time is 1～3h;
(3) thermomechanical processing: the ingot blank through above-mentioned hip treatment carries out hot rolling cogging, and rolling temperature is 800～1100 ℃, carries out transverse and longitudinal and replaces rolling, and the pass deformation of rolling is not more than 10%;
(4) cold mechanical workout: the blank through the processing of above-mentioned thermomechanical need carry out cold rolling and final mechanical workout moulding, described cold rolling longitudinal rolling that is made as, the pass deformation of rolling is not more than 5%.
In described vacuum induction melting process, before casting, need there is the process of setting of twice, setting time is not less than 5 minutes for the first time, and the time of solidifying is for the second time not less than 15 minutes.
Also comprise operation prepared by CoB master alloy.
Magnetic recording media prepared by a kind of CoCrPt of use based alloy sputtering target material, described magnetic recording media comprises stratum basale, tack coat, soft magnetosphere, middle layer and magnetic recording layer, the coercive force of described magnetic recording media is 3000～5000Oe, squareness is 0.80～095, particle size 4～the 10nm of described magnetic recording layer, roughness of film is 2～5nm.
The present invention is by adjusting vacuum melting casting mode and cold and hot working rolling mode and pass deformation, and increase hot isostatic pressing operation etc., prepare a kind of CoCrPt based alloy sputtering target material, this target detrimental impurity constituent content is low, grain-size is tiny evenly, Chemical Composition evenly and to depart from nominal composition less, the method has solved rolling crack in conventional preparation technology, yield rate is low, it is more that alloy target material target Chemical Composition departs from nominal composition, the technical problems such as detrimental impurity content is higher, the magnetic recording media crystal grain that uses this sputtering target material to prepare is tiny evenly, non magnetic crystal boundary is obvious, magnetic performance is good.
Accompanying drawing explanation
Fig. 1 is the BE-SEM pattern of Co11.5Cr22Pt10B alloy sputtering target in comparative example;
Fig. 2 is that each element that the EPMA of Co11.5Cr22Pt10B sputtering target material of the present invention analyzes distributes;
Co11.5Cr22Pt10B alloy rolling cracking photomacrograph in Fig. 3 comparative example 3;
Fig. 4 is for being used the AFM figure of the magnetic recording media magnetic recording layer of Co11.5Cr11Pt10B sputtering target material formation of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further illustrated, but never in any form the present invention is limited, and any change or the improvement based on training centre of the present invention, done, all belong to protection scope of the present invention.
CoCrPt based alloy sputtering target material of the present invention also comprises B element, the content of described B element is 0～20 atomic percent, described alloy target material comprises rich Co phase and rich B two thing phases mutually, wherein rich B be evenly distributed in mutually rich Co mutually in, the average grain size of described rich Co phase is at 20～50 μ m, and the average grain size of rich B phase is at 0～20 μ m.
Described alloy target material is Co11.5Cr22Pt10B or Co13Cr16Pt10B.
Described alloy target material also comprises Si, Ti, Ta, Y, one or more in the elements such as Zr.
The actual content of described each element of alloy target material and the deviation <0.5at% of nominal content.
The C content <50ppm of described alloy target material, O content <50ppm, S content <10ppm, N content <10ppm.
The coercive force of described alloy sputtering target is at 3500～4500Oe, and described alloy target material thickness is when the thickness of 4～9mm, and its magnetic susceptibility is between 50%～80%.
The method of CoCrPt based alloy sputtering target material of the present invention, comprising:
(1) vacuum melting: material is prepared burden by stoichiometric ratio, described vacuum melting is intermediate frequency vacuum induction melting, institute's use crucible for aluminum oxide or zirconium white crucible, pouring temperature be 1500～1650 ℃, before casting, melt includes the process of setting of at least 1 time in crucible;
(2) hot isostatic pressing: described ingot casting need pass through hip treatment, 800～1100 ℃ of temperature, 4N high-purity Ar atmosphere, pressure is 150～200MPa, soaking time is 1～3h;
(3) thermomechanical processing: the ingot blank through above-mentioned hip treatment carries out hot rolling cogging, and rolling temperature is 800～1100 ℃, carries out transverse and longitudinal and replaces rolling, and the pass deformation of rolling is not more than 10%;
(4) cold mechanical workout: the blank through the processing of above-mentioned thermomechanical need carry out cold rolling and final mechanical workout moulding, described cold rolling longitudinal rolling that is made as, the pass deformation of rolling is not more than 5%.
In described vacuum induction melting process, before casting, need there is the process of setting of twice, setting time is not less than 5 minutes for the first time, and the time of solidifying is for the second time not less than 15 minutes.
Also comprise operation prepared by CoB master alloy.
Magnetic recording media prepared by a kind of CoCrPt of use based alloy sputtering target material, described magnetic recording media comprises stratum basale, tack coat, soft magnetosphere, middle layer and magnetic recording layer, the coercive force of described magnetic recording media is 3000～5000Oe, squareness is 0.80～095, particle size 4～the 10nm of described magnetic recording layer, roughness of film is 2～5nm.
Below in conjunction with specific embodiment to the based alloy sputtering target material of CoCrPt described in the present invention, preparation method with and magnetic recording media be specifically described.
Embodiment 1
Co11.5Cr22Pt10B sputtering target material of the present invention is prepared as follows:
(1) raw material is prepared: select Co more than 3N5, and Cr, the B of Pt and C content <100ppm is as raw material;
(2) master alloy preparation: adopt vacuum induction melting method to prepare Co according to the nominal content of alloy
80b
20the master alloy of (atomic percent);
(3) preparation of alloy cast ingot: use above-mentioned master alloy, prepare burden according to nominal composition Co11.5Cr22Pt10B, adopt vacuum induction melting method to prepare alloy cast ingot, be first evacuated down to 1 * 10
-1below Pa, then heat up gradually and start melting materials capable, after material all melts, logical argon gas, stops heating, starts to solidify material, solidifies approximately 5～20min, then continues to heat up, and after the whole fusings of material, ingot casting is poured in mould;
(4) hip treatment: at 800～1000 ℃, 100～200MPa, carries out hip treatment to ingot casting under the above high-purity argon gas protection of the environment of 3N5, and the treatment time is 1～5h;
(5) cold and hot mechanical workout: the ingot casting after above-mentioned processing is carried out to hot rolling at 900～1100 ℃, and the pass deformation of rolling is 5%～8%, the total deflection of hot rolling is 40%～50%, carries out transverse and longitudinal and replace rolling in the operation of rolling; Blank after hot rolling is carried out to cold-rolling treatment, and the pass deformation of rolling is 3%～5%, and cold rolling total deflection is 20～30%, and the most above-mentioned blank is worked into required product size.
In magnetron sputtering equipment, use the magnetic recording layer of the preparation of target materials magnetic recording media of above-mentioned preparation.
Comparative example 1
Difference from Example 1 is Co more than 3N5, Cr, and Pt and common B powder are directly prepared burden and are carried out vacuum induction melting as raw material.
Comparative example 2
Difference from Example 1 is that described Co11.5Cr22Pt10B ingot casting has not carried out process of setting direct fusion and poured into a mould in fusion process.
Comparative example 3
Difference from Example 1 is that described Co11.5Cr22Pt10B ingot casting does not carry out hip treatment and directly carries out cold and hot mechanical workout.
By ICP-OES, carry out principal component analysis, adopt LECO-CS230 and TC400 respectively C, S and N, O to be analyzed, adopt SEM and EPMA to characterize alloy target material heterogeneous microstructure, the magnetic spectroscopy susceptibility of measuring alloy target material according to ASTMF1761-00 (2011) standard method of test is PTF; Simultaneously, use method sputter ruthenium-base alloy film on Si (100) sheet of magnetron sputtering, by vibrating sample magnetometer (VSM), the magnetism characteristic of thin film dielectrics is characterized, adopt atomic force microscope (AFM) to characterize the structure of magnetic recording layer in magnetic recording media.
As shown in table 1～2, embodiment 1 relatively finds with comparative example 1, does not use CoB master alloy directly to carry out melting, is easy to cause the volatilization of B element, causes B content to depart from nominal composition, uses common B powder simultaneously, can cause C in ingot casting, O content overproof; Embodiment 1 relatively finds with comparative example 2, after the whole fusings of material, solidifies processing, finally causes O in ingot casting, and N content is higher, and visible process of setting can cause O, the reduction of the gas contents such as N; As shown in Figure 1, do not carry out hip treatment, because inside ingot exists founding defect, the fragility of alloy material own is higher simultaneously, finally causes ingot blank in hot rolling cogging process very easily to ftracture, and reduces the yield rate of product.
As shown in table 3～4, the target of not processing through cold and hot working, magnetic spectroscopy susceptibility (PTF) is all below 40%, and inhomogeneous everywhere, differ 20% left and right, cause the not starting the arc in magnetron sputtering process cannot realize spatter film forming, and after processing by cold and hot working, its PTF value of target of preparation is even, all more than 70%, and deviation is in 5%.High and surface particles size uniform is tiny by the magneticthin film coercive force of this preparation of target materials.
Table 1 Chemical Composition comparison (at%)
Table 2 C, N, O content comparison (ppm)
| Element | Embodiment 1 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| C | 39 | 160 | 45 | 40 |
| S | <10 | 45 | 10 | <10 |
| O | 45 | 300 | 280 | 42 |
| N | <10 | 50 | 90 | <10 |
Table 3 PTF observed value
| Test point | Embodiment 1 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Spot1 | 75％ | 25％ | 25％ | 20％ |
| Spot2 | 72％ | 35％ | 30％ | 45％ |
| Spot3 | 74％ | 20％ | 25％ | 30％ |
| Spot4 | 75％ | 40％ | 40％ | 40％ |
Note: it is 114.3mm that target size is diameter, and 5.08mm is thick, the target in comparative example 1～3, by grinding machine processing preparation after the cutting of ingot casting line, is got clockwise interval 90 degree and is got four point measurement PTF values.
Table 6 magnetic recording media Performance Ratio
| Performance | Embodiment 1 | Comparative example 1 | Embodiment 2 | Embodiment 3 |
| Coercive force (Oe) | 4500 | The not starting the arc | The not starting the arc | The not starting the arc |
| Squareness (Hc/) | 0.9 | The not starting the arc | The not starting the arc | The not starting the arc |
| Average particle size particle size (magnetic recording layer) | 8nm | The not starting the arc | The not starting the arc | The not starting the arc |
| Surface roughness Ra (magnetic recording layer) | 4nm | The not starting the arc | The not starting the arc | The not starting the arc |
In sum, the present invention (prepares ingot casting as used master alloy by adjusting vacuum melting casting mode, in the middle of increasing melting, solidify link etc.) and cold and hot working rolling mode and pass deformation, and increase hot isostatic pressing operation etc., prepare a kind of CoCrPt based alloy sputtering target material, this target obnoxious flavour impurity content is low, grain-size is tiny evenly, Chemical Composition evenly and to depart from nominal composition less, the method has solved rolling crack in conventional preparation technology, yield rate is low, it is more that alloy target material Chemical Composition departs from nominal composition, the technical problems such as detrimental impurity content is higher, the magnetic recording media crystal grain that uses this sputtering target material to prepare is tiny evenly, non magnetic crystal boundary is obvious, magnetic performance is good.
Claims (10)
1. a CoCrPt based alloy sputtering target material, it is characterized in that: described CoCrPt based alloy sputtering target material contains B element, the content of B element is 0～20 atomic percent, described alloy target material comprises rich Co phase and rich B two thing phases mutually, wherein rich B be evenly distributed in mutually rich Co mutually in, the average grain size of described rich Co phase is at 20～50 μ m, and the average grain size of rich B phase is at 0～20 μ m.
2. CoCrPt based alloy sputtering target material according to claim 1, is characterized in that: described alloy target material is Co11.5Cr22Pt10B or Co13Cr16Pt10B.
3. CoCrPt based alloy sputtering target material according to claim 1, is characterized in that: described alloy target material also contains Si, Ti, Ta, Y, one or more in the elements such as Zr.
4. CoCrPt based alloy sputtering target material according to claim 1, is characterized in that: the actual content of described each element of alloy target material and the deviation <0.5at% of nominal content.
5. CoCrPt based alloy sputtering target material according to claim 1, it is characterized in that: the C content <50ppm of described alloy target material, O content <50ppm, S content <10ppm, N content <10ppm.
6. CoCrPt based alloy sputtering target material according to claim 1, is characterized in that: the coercive force of described alloy sputtering target is at 3500～4500Oe, and described alloy target material thickness is when the thickness of 4～9mm, and its magnetic susceptibility is between 50%～80%.
7. a method of preparing CoCrPt based alloy sputtering target material claimed in claim 1, comprising:
(1) vacuum melting: material is prepared burden by stoichiometric ratio, described CoCrPt based alloy sputtering target material contains B element, the content of B element is 0～20 atomic percent, vacuum melting is intermediate frequency vacuum induction melting, institute's use crucible is aluminum oxide or zirconium white crucible, pouring temperature is 1500～1650 ℃, and before casting, melt includes the process of setting of at least 1 time in crucible;
(2) hot isostatic pressing: described ingot casting need pass through hip treatment, 800～1100 ℃ of temperature, 4N high-purity Ar atmosphere, pressure is 150～200MPa, soaking time is 1～3h;
(3) thermomechanical processing: the ingot blank through above-mentioned hip treatment carries out hot rolling cogging, and rolling temperature is 800～1100 ℃, carries out transverse and longitudinal and replaces rolling, and the pass deformation of rolling is not more than 10%;
(4) cold mechanical workout: the blank through the processing of above-mentioned thermomechanical need carry out cold rolling and final mechanical workout moulding, described cold rolling longitudinal rolling that is made as, the pass deformation of rolling is not more than 5%.
8. the preparation method of CoCrPt based alloy sputtering target material according to claim 7, is characterized in that: also comprise operation prepared by CoB master alloy;
Described CoCrPt alloy target material is Co11.5Cr22Pt10B or Co13Cr16Pt10B, and described alloy target material also contains Si, Ti, and Ta, Y, one or more in the elements such as Zr,
In described vacuum induction melting process, before casting, need there is the process of setting of twice, setting time is not less than 5 minutes for the first time, and the time of solidifying is for the second time not less than 15 minutes.
9. a preparation method for Co11.5Cr22Pt10B sputtering target material, is characterized in that containing following processing step:
(1) raw material is prepared: select Co more than 3N5, and Cr, the B of Pt and C content <100ppm is as raw material; (2) master alloy preparation: adopt vacuum induction melting method to prepare Co according to the nominal content of alloy
80b
20the master alloy of (atomic percent);
(3) preparation of alloy cast ingot: use above-mentioned master alloy, prepare burden according to nominal composition Co11.5Cr22Pt10B, adopt vacuum induction melting method to prepare alloy cast ingot, be first evacuated down to 1 * 10
-1below Pa, then heat up gradually and start melting materials capable, after material all melts, logical argon gas, stops heating, starts to solidify material, solidifies approximately 5～20min, then continues to heat up, and after the whole fusings of material, ingot casting is poured in mould;
(4) hip treatment: at 800～1000 ℃, 100～200MPa, carries out hip treatment to ingot casting under the above high-purity argon gas protection of the environment of 3N5, and the treatment time is 1～5h;
(5) cold and hot mechanical workout: the ingot casting after above-mentioned processing is carried out to hot rolling at 900～1100 ℃, and the pass deformation of rolling is 5%～8%, the total deflection of hot rolling is 40%～50%, carries out transverse and longitudinal and replace rolling in the operation of rolling; Blank after hot rolling is carried out to cold-rolling treatment, and the pass deformation of rolling is 3%～5%, and cold rolling total deflection is 20～30%, and the most above-mentioned blank is worked into required product size.
10. the magnetic recording media that prepared by the CoCrPt based alloy sputtering target material described in a right to use requirement 1, described magnetic recording media comprises stratum basale, tack coat, soft magnetosphere, middle layer and magnetic recording layer, is characterized in that: the coercive force of described magnetic recording media is 3000～5000Oe, and squareness is 0.80～095, particle size 4～the 10nm of described magnetic recording layer, roughness of film is 2～5nm.
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| CN111876737A (en) * | 2020-07-24 | 2020-11-03 | 宁波江丰电子材料股份有限公司 | Nickel-chromium alloy sputtering target material and preparation method thereof |
| CN114293159A (en) * | 2021-12-15 | 2022-04-08 | 先导薄膜材料（广东）有限公司 | Preparation method of nickel-based alloy target material |
| CN114293159B (en) * | 2021-12-15 | 2024-01-19 | 先导薄膜材料（广东）有限公司 | Preparation method of nickel-based alloy target |
| CN115747732A (en) * | 2022-11-21 | 2023-03-07 | 先导薄膜材料（广东）有限公司 | CoFeSiB alloy target and preparation method thereof |
| CN115747732B (en) * | 2022-11-21 | 2024-08-30 | 先导薄膜材料（广东）有限公司 | CoFeSiB alloy target and preparation method thereof |
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