CN104032274B - A kind of CoCrPt based alloy sputtering target material and thin film and preparation method thereof - Google Patents
A kind of CoCrPt based alloy sputtering target material and thin film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of CoCrPt based alloy sputtering target material and thin film and preparation method thereof, described CoCrPt based alloy sputtering target material includes B element, the content of B element is 0～20 atomic percent, described alloy target material includes rich Co phase and rich two thing phases of B phase, wherein rich B phase is evenly distributed in rich Co phase, the average grain size of described rich Co phase is at 20～50 μm, and the average grain size of rich B phase is at 0～20 μm；The preparation method of described CoCrPt based alloy sputtering target material, including: (1) vacuum melting；(2) high temperature insostatic pressing (HIP)；(3) thermomechanical processing；(4) cold machining.Using magnetic recording media prepared by CoCrPt based alloy sputtering target material of the present invention, described magnetic recording media includes basal layer, tack coat, soft magnetosphere, intermediate layer and magnetic recording layer, the coercivity of described magnetic recording media is 3000～5000Oe, and squareness is 0.80～095.Chemical analysis of the present invention is uniform and deviation nominal composition is less, solves rolling crack in conventional fabrication process, and yield rate is low, the alloy target material chemical analysis deviation name technical problems such as composition is more, objectionable impurities content is higher.
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, thin film and preparation method thereof.
Background technology
1970, the material that Japan's professor's rock rugged pretty uses when proposing perpendicular magnetic recording medium was CoCr alloy, and the originally research of people collects in just in CoCrX alloy, and wherein X material is typically chosen as Ta, Pt, Nb, B etc..Pt can strengthen the magnetocrystalline anisotropy of CoCr material；Cr is easier from crystal grain to precipitate out the grain boundary forming rich Cr, interacts thus reducing intercrystalline exchange conjunction；Add Ta and be conducive to the precipitation of Cr；B is easier to from crystal grain to precipitate out than Cr, thus effectively reducing intercrystalline coupling.Therefore, CoCrPtB alloy sputtering target is widely used as the magnetic recording layer in hard disk or coupling layer.
But the interpolation due to B element so that the fragility of the CoCrPt system alloy that original fragility is bigger is bigger, and room temperature elongation percentage, less than 2%, therefore prepares such alloy sputtering target only by hot worked mode.Patent documentation 1 (US7927434) discloses a kind of CoCrPtB alloy sputtering target and preparation method thereof, the method prepares ingot blank by vacuum induction melting method, subsequently at 1100 DEG C of these ingot blanks of hot rolling, require that its heat distortion amount is between 15～40%, obtain coercivity alloy target material between 3282～3293Oe, and its crystallite dimension is below 200 microns.It is repeated experiment and finds by the present inventor: (1) uses merely tetra-kinds of materials of Co, Cr, Pt, B stoichiometrically to carry out dispensing to carry out induction melting, and owing to B is readily volatilized, the chemical composition of final ingot blank can deviate name formulated component；(2) can there is the founding defects such as pore unavoidably in inside ingot prepared by vacuum induction melting, due to the fragility of CoCrPtB alloy itself, even if at the course of hot rolling of 1100 DEG C, defect also can extend, form crackle, ultimately result in ingot blank brisement, thus the yield rate of product is greatly reduced.
Patent documentation 2 (US6797137) discloses a kind of CoCrPtB alloy sputtering target and preparation method thereof, alloy target material is prepared mainly by powder metallurgic method, the mechanical properties such as the elongation percentage of the alloy target material of preparation and fracture characteristics all make moderate progress, but it is owing to powder metallurgic method requires over the operation such as powder process, ball milling, compressing eventually through the mode such as vacuum hotpressing or high temperature insostatic pressing (HIP).Therefore have following defects that compared with smelting process that (1) chemical composition uniformity is poor；(2) target gas content is higher, and consistency prepares target lower than smelting process；(3) in order to uniform ingredients to carry out long ball milling mixed processing, it is easy to introduce impurity.Disadvantages mentioned above ultimately results in film composition lack of homogeneity, and film thickness uniformity is poor, and thin film is easily generated the ill effects such as defect, finally affects the magnetism characteristic of thin film.
Based on above Problems existing, present inventors have proposed a kind of chemical analysis and uniformly and deviate name CoCrPtB alloy sputtering target that composition is less, crystallite dimension fine uniform, impurity content are low and preparation method thereof, the method not only ensures that the chemical analysis of the said goods is uniform, impurity content is low, but also finished product rate can be improved, additionally provide the magnetic recording media of a kind of thus preparation of target materials simultaneously, the magnetic recording layer surface particles fine uniform of this magnetic recording media, coercivity is high, and squareness is good.
Summary of the invention
It is an object of the invention to provide a kind of CoCrPt based alloy sputtering target material and thin film and preparation method thereof, described sputtering target, objectionable impurities constituent content is low, crystallite dimension fine uniform, and chemical analysis is uniform and deviation nominal composition is less.
Another object of the present invention is to provide a kind of thin film magnetic recording media using above-mentioned sputtering target material to prepare, this magnetic recording media uniform small grains, non magnetic crystal boundary are obvious, and magnetic performance is excellent.
The first object of the present invention is realized in, described CoCrPt based alloy sputtering target material also includes B element, the content of described B element is 0～20 atomic percent, described alloy target material includes rich Co phase and rich two thing phases of B phase, wherein rich B phase is evenly distributed in rich Co phase, the average grain size of described rich Co phase is at 20～50 μm, and the average grain size of rich B phase is at 0～20 μm.
Described alloy target material is Co11.5Cr22Pt10B or Co13Cr16Pt10B.
Described alloy target material also includes one or more in the elements such as Si, Ti, Ta, Y, Zr.
Deviation < the 0.5at% of the actual content of each element of described alloy target material and name content.
C content < 50ppm, O content < 50ppm, S content < 10ppm, N content < 10ppm of described alloy target material.
The coercivity 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 kind of method preparing described CoCrPt based alloy sputtering target material, including:
(1) vacuum melting: material is stoichiometrically carried out dispensing, described vacuum melting is intermediate frequency vacuum induction melting, and institute's use crucible is aluminium oxide or zirconium oxide crucible, and cast temperature is 1500～1650 DEG C, before casting, melt includes the process of setting of at least 1 time in crucible；
(2) high temperature insostatic pressing (HIP): described ingot casting need to through hip treatment, temperature 800～1100 DEG C, 4N high-purity Ar atmosphere, and pressure is 150～200MPa, and temperature retention 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 DEG C, carries out transverse and longitudinal alternately rolling, and the pass deformation of rolling is not more than 10%；
(4) cold machining: the blank processed through above-mentioned thermomechanical need to carry out cold rolling and final machining molding, described cold rolling is made as longitudinal rolling, and the pass deformation of rolling is not more than 5%.
Needing the process of setting of twice in described vacuum induction melting process before casting, first time setting time is not less than 5 minutes, and the time of second time solidification is not less than 15 minutes.
Also include operation prepared by CoB intermediate alloy.
Magnetic recording media prepared by a kind of CoCrPt of use based alloy sputtering target material, described magnetic recording media includes basal layer, tack coat, soft magnetosphere, intermediate layer and magnetic recording layer, the coercivity 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.
The present invention is by adjusting vacuum melting casting mode and cold and hot working rolling mode and pass deformation, and increase high temperature insostatic pressing (HIP) operation etc., prepare a kind of CoCrPt based alloy sputtering target material, this target objectionable impurities constituent content is low, crystallite dimension fine uniform, chemical analysis is uniform and deviation nominal composition is less, this method solve rolling crack in conventional fabrication process, yield rate is low, alloy target material target chemical analysis deviation name composition is more, the technical problems such as objectionable impurities content is higher, use magnetic recording media uniform small grains prepared by this sputtering target material, non magnetic crystal boundary is obvious, magnetic performance is excellent.
Accompanying drawing explanation
Fig. 1 is the BE-SEM pattern of Co11.5Cr22Pt10B alloy sputtering target in comparative example；
Fig. 2 is each Elemental redistribution of the EPMA analysis of Co11.5Cr22Pt10B sputtering target material of the present invention；
Co11.5Cr22Pt10B alloy rolling cracking photomacrograph in Fig. 3 comparative example 3；
Fig. 4 is the AFM figure of the magnetic recording media magnetic recording layer using Co11.5Cr11Pt10B sputtering target material of the present invention to be formed.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is further illustrated, but never in any form the present invention is any limitation as, and based on present invention teach that any change or improvement made, belongs to protection scope of the present invention.
CoCrPt based alloy sputtering target material of the present invention also includes B element, the content of described B element is 0～20 atomic percent, described alloy target material includes rich Co phase and rich two thing phases of B phase, wherein rich B phase is evenly distributed in rich Co phase, the average grain size of described rich Co phase is at 20～50 μm, and the average grain size of rich B phase is at 0～20 μm.
Described alloy target material is Co11.5Cr22Pt10B or Co13Cr16Pt10B.
Described alloy target material also includes one or more in the elements such as Si, Ti, Ta, Y, Zr.
Deviation < the 0.5at% of the actual content of each element of described alloy target material and name content.
C content < 50ppm, O content < 50ppm, S content < 10ppm, N content < 10ppm of described alloy target material.
The coercivity 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, including:
(1) vacuum melting: material is stoichiometrically carried out dispensing, described vacuum melting is intermediate frequency vacuum induction melting, and institute's use crucible is aluminium oxide or zirconium oxide crucible, and cast temperature is 1500～1650 DEG C, before casting, melt includes the process of setting of at least 1 time in crucible；
(2) high temperature insostatic pressing (HIP): described ingot casting need to through hip treatment, temperature 800～1100 DEG C, 4N high-purity Ar atmosphere, and pressure is 150～200MPa, and temperature retention 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 DEG C, carries out transverse and longitudinal alternately rolling, and the pass deformation of rolling is not more than 10%；
(4) cold machining: the blank processed through above-mentioned thermomechanical need to carry out cold rolling and final machining molding, described cold rolling is made as longitudinal rolling, and the pass deformation of rolling is not more than 5%.
Needing the process of setting of twice in described vacuum induction melting process before casting, first time setting time is not less than 5 minutes, and the time of second time solidification is not less than 15 minutes.
Also include operation prepared by CoB intermediate alloy.
Magnetic recording media prepared by a kind of CoCrPt of use based alloy sputtering target material, described magnetic recording media includes basal layer, tack coat, soft magnetosphere, intermediate layer and magnetic recording layer, the coercivity 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.
Below in conjunction with specific embodiment, heretofore described CoCrPt based alloy sputtering target material, preparation method and its magnetic recording media are specifically described.
Embodiment 1
Co11.5Cr22Pt10B sputtering target material of the present invention is prepared as follows:
(1) raw material prepares: < B of 100ppm is as raw material for Co, Cr, the Pt of selection more than 3N5 and C content；
(2) prepared by intermediate alloy: adopt vacuum induction melting method to prepare Co according to the nominal content of alloy80B20The intermediate alloy of (atomic percent)；
(3) preparation of alloy cast ingot: use above-mentioned intermediate alloy, carries out dispensing according to name composition Co11.5Cr22Pt10B, adopts vacuum induction melting method to prepare alloy cast ingot, is first evacuated down to 1 × 10-1Below Pa, then heats up gradually and starts melting materials, after material all melts, and logical argon, stop heating, start to solidify material, solidify about 5～20min, then proceed to heat up, after material all melts, ingot casting is poured in mould；
(4) hip treatment: at 800～1000 DEG C, 100～200MPa, under more than 3N5 high-purity argon gas protection environment, ingot casting is carried out hip treatment, the process time is 1～5h；
(5) cold and hot machining: at 900～1100 DEG C, the ingot casting after above-mentioned process is carried out hot rolling, the pass deformation of rolling is 5%～8%, and the total deflection of hot rolling is 40%～50%, carries out transverse and longitudinal alternately rolling in the operation of rolling；Blank after hot rolling is carried out 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.
Magnetron sputtering apparatus uses 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 in that as raw material direct dispensing, Co, Cr, Pt and the common B powder of more than 3N5 are carried out vacuum induction melting.
Comparative example 2
Difference from Example 1 is in that described Co11.5Cr22Pt10B ingot casting does not carry out process of setting direct fusion in fusion process and pours into a mould.
Comparative example 3
Difference from Example 1 is in that described Co11.5Cr22Pt10B ingot casting does not carry out hip treatment and is made directly cold and hot machining.
Principal component analysis is carried out by ICP-OES, LECO-CS230 and TC400 is adopted respectively C, S and N, O to be analyzed, adopt SEM and EPMA to characterize alloy target material heterogeneous microstructure, measure magnetic spectroscopy susceptibility and the PTF of alloy target material according to ASTMF1761-00 (2011) standard method of test；Simultaneously, the method using magnetron sputtering sputters ruthenium-base alloy thin film on Si (100) sheet, by vibrating specimen magnetometer (VSM), the magnetism characteristic of thin film dielectrics is characterized, adopt atomic force microscope (AFM) that the structure of magnetic recording layer in magnetic recording media is characterized.
As shown in table 1～2, embodiment 1 compares discovery with comparative example 1, does not use CoB intermediate alloy to be made directly melting, it is easy to cause the volatilization of B element, causes B content deviation name composition, uses common B powder simultaneously, can cause C in ingot casting, and O content exceeds standard；Embodiment 1 compares discovery with comparative example 2, and material does not carry out solidification process after all melting, and ultimately results in O in ingot casting, and N content is higher, it is seen that process of setting can cause the reduction of the gas contents such as O, N；As it is shown in figure 1, do not carry out hip treatment, owing to inside ingot exists founding defect, the fragility of alloy material own is higher simultaneously, ultimately results in ingot blank in hot rolling cogging process and very easily ftractures, and reduces the yield rate of product.
As shown in table 3～4, without the target that cold and hot working processes, magnetic spectroscopy susceptibility (PTF) is all below 40%, and it is uneven everywhere, difference about 20%, causes that the not starting the arc cannot realize spatter film forming in magnetron sputtering process, and after being processed by cold and hot working, its PTF value of target of preparation is uniform, all more than 70%, and deviation is within 5%.Tiny by the thin magnetic film coercivity of this preparation of target materials height and surface particles size uniform.
Table 1 chemical analysis compares (at%)
Table 2C, N, O content compares (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 3PTF measured 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, 5.08mm thickness that target size is diameter, the target in comparative example 1～3, by grinding machine processing preparation after ingot casting line is cut, takes 90 degree of interval clockwise and takes four somes measurement PTF values.
Table 6 magnetic recording media Performance comparision
| Performance | Embodiment 1 | Comparative example 1 | Embodiment 2 | Embodiment 3 |
| Coercivity (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 is by adjusting vacuum melting casting mode (as used intermediate alloy to prepare ingot casting, increase melting intermediate setup link etc.) and cold and hot working rolling mode and pass deformation, and increase high temperature insostatic pressing (HIP) operation etc., prepare a kind of CoCrPt based alloy sputtering target material, this target harmful gaseous impurities constituent content is low, crystallite dimension fine uniform, chemical analysis is uniform and deviation nominal composition is less, this method solve rolling crack in conventional fabrication process, yield rate is low, alloy target material chemical analysis deviation name composition is more, the technical problems such as objectionable impurities content is higher, use magnetic recording media uniform small grains prepared by this sputtering target material, non magnetic crystal boundary is obvious, magnetic performance is excellent.
Claims (3)
1. the method preparing CoCrPt based alloy sputtering target material, including:
(1) vacuum melting: material is stoichiometrically carried out dispensing, described CoCrPt based alloy sputtering target material contains B element, the content of B element is 0～20 atomic percent, described alloy target material includes rich Co phase and rich two thing phases of B phase, wherein rich B phase is evenly distributed in rich Co phase, the average grain size of described rich Co phase is at 20～50 μm, the average grain size of rich B phase is at 0～20 μm, vacuum melting is intermediate frequency vacuum induction melting, institute's use crucible is aluminium oxide or zirconium oxide crucible, cast temperature is 1500～1650 DEG C, before casting, melt includes the process of setting of at least 1 time in crucible；
(2) hip treatment: temperature 800～1100 DEG C, 4N high-purity Ar atmosphere, pressure is 150～200MPa, and temperature retention 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 DEG C, carries out transverse and longitudinal alternately rolling, and the pass deformation of rolling is not more than 10%；
(4) cold machining: the blank processed through above-mentioned thermomechanical need to carry out cold rolling and final machining molding, described cold rolling is made as longitudinal rolling, and the pass deformation of rolling is not more than 5%.
2. the preparation method of CoCrPt based alloy sputtering target material according to claim 1, it is characterised in that: also include operation prepared by CoB intermediate alloy；
Described CoCrPt alloy target material is Co11.5Cr22Pt10B or Co13Cr16Pt10B, described alloy target material possibly together with one or more in Si, Ti, Ta, Y, Zr element,
Needing the process of setting of twice in described vacuum induction melting process before casting, first time setting time is not less than 5 minutes, and the time of second time solidification is not less than 15 minutes.
3. the preparation method of a Co11.5Cr22Pt10B sputtering target material, it is characterised in that containing following processing step:
(1) raw material prepares: < B of 100ppm is as raw material for Co, Cr, the Pt of selection more than 3N5 and C content；
(2) prepared by intermediate alloy: adopt vacuum induction melting method to prepare Co according to the nominal content of alloy80B20The intermediate alloy of atomic percent；
(3) preparation of alloy cast ingot: use above-mentioned intermediate alloy, carries out dispensing according to name composition Co11.5Cr22Pt10B, adopts vacuum induction melting method to prepare alloy cast ingot, is first evacuated down to 1 × 10-1Below Pa, then heats up gradually and starts melting materials, after material all melts, and logical argon, stop heating, start to solidify material, solidify 5～20min, then proceed to heat up, after material all melts, ingot casting is poured in mould；
(4) hip treatment: at 800～1000 DEG C, 100～200MPa, under more than 3N5 high-purity argon gas protection environment, ingot casting is carried out hip treatment, the process time is 1～5h；
(5) cold and hot machining: at 900～1100 DEG C, the ingot casting after above-mentioned process is carried out hot rolling, the pass deformation of rolling is 5%～8%, and the total deflection of hot rolling is 40%～50%, carries out transverse and longitudinal alternately rolling in the operation of rolling；Blank after hot rolling is carried out 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.
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| CN111218630A (en) * | 2020-03-11 | 2020-06-02 | 宁波江丰电子材料股份有限公司 | Method for eliminating defects of ultrahigh-purity copper ingot |
| 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 |
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| US6797137B2 (en) * | 2001-04-11 | 2004-09-28 | Heraeus, Inc. | Mechanically alloyed precious metal magnetic sputtering targets fabricated using rapidly solidfied alloy powders and elemental Pt metal |
| JP4026767B2 (en) * | 2003-11-11 | 2007-12-26 | 日鉱金属株式会社 | Co-Cr-Pt-B alloy sputtering target and method for producing the same |
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