TWI838846B - Fe-pt based sputtering target and method of preparing the same - Google Patents
Fe-pt based sputtering target and method of preparing the same Download PDFInfo
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- TWI838846B TWI838846B TW111133336A TW111133336A TWI838846B TW I838846 B TWI838846 B TW I838846B TW 111133336 A TW111133336 A TW 111133336A TW 111133336 A TW111133336 A TW 111133336A TW I838846 B TWI838846 B TW I838846B
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- iron
- platinum
- nitride
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- based target
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- 238000005477 sputtering target Methods 0.000 title abstract description 12
- 238000004544 sputter deposition Methods 0.000 title description 20
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 48
- 150000004767 nitrides Chemical class 0.000 claims abstract description 45
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 33
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 27
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 15
- 229910052742 iron Inorganic materials 0.000 claims abstract description 12
- 229910052796 boron Inorganic materials 0.000 claims abstract description 8
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 7
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 7
- 229910052741 iridium Inorganic materials 0.000 claims abstract description 6
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 6
- 229910052703 rhodium Inorganic materials 0.000 claims abstract description 6
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 6
- OBACEDMBGYVZMP-UHFFFAOYSA-N iron platinum Chemical compound [Fe].[Fe].[Pt] OBACEDMBGYVZMP-UHFFFAOYSA-N 0.000 claims description 138
- 239000002994 raw material Substances 0.000 claims description 103
- 238000005245 sintering Methods 0.000 claims description 49
- 239000000203 mixture Substances 0.000 claims description 47
- 239000013077 target material Substances 0.000 claims description 41
- 239000011575 calcium Substances 0.000 claims description 33
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 32
- 239000001301 oxygen Substances 0.000 claims description 32
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 31
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 28
- 229910052799 carbon Inorganic materials 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 21
- 239000001257 hydrogen Substances 0.000 claims description 21
- 229910052739 hydrogen Inorganic materials 0.000 claims description 21
- 238000005406 washing Methods 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 16
- 230000009467 reduction Effects 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 13
- -1 nickel nitride Chemical class 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- UNASZPQZIFZUSI-UHFFFAOYSA-N methylidyneniobium Chemical compound [Nb]#C UNASZPQZIFZUSI-UHFFFAOYSA-N 0.000 claims description 8
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 8
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000011946 reduction process Methods 0.000 claims description 7
- 229910052707 ruthenium Inorganic materials 0.000 claims description 7
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 6
- 229910052785 arsenic Inorganic materials 0.000 claims description 6
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 6
- RRZKHZBOZDIQJG-UHFFFAOYSA-N azane;manganese Chemical compound N.[Mn] RRZKHZBOZDIQJG-UHFFFAOYSA-N 0.000 claims description 6
- SKKMWRVAJNPLFY-UHFFFAOYSA-N azanylidynevanadium Chemical compound [V]#N SKKMWRVAJNPLFY-UHFFFAOYSA-N 0.000 claims description 6
- 239000010955 niobium Substances 0.000 claims description 6
- 239000010948 rhodium Substances 0.000 claims description 6
- INZDTEICWPZYJM-UHFFFAOYSA-N 1-(chloromethyl)-4-[4-(chloromethyl)phenyl]benzene Chemical compound C1=CC(CCl)=CC=C1C1=CC=C(CCl)C=C1 INZDTEICWPZYJM-UHFFFAOYSA-N 0.000 claims description 5
- 229910052582 BN Inorganic materials 0.000 claims description 5
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 5
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 5
- 229910026551 ZrC Inorganic materials 0.000 claims description 5
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 claims description 5
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 5
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 5
- 229910003470 tongbaite Inorganic materials 0.000 claims description 5
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims description 5
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 5
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 5
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 claims description 4
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- GPBUGPUPKAGMDK-UHFFFAOYSA-N azanylidynemolybdenum Chemical compound [Mo]#N GPBUGPUPKAGMDK-UHFFFAOYSA-N 0.000 claims description 4
- CFJRGWXELQQLSA-UHFFFAOYSA-N azanylidyneniobium Chemical compound [Nb]#N CFJRGWXELQQLSA-UHFFFAOYSA-N 0.000 claims description 4
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 4
- UFGZSIPAQKLCGR-UHFFFAOYSA-N chromium carbide Chemical compound [Cr]#C[Cr]C#[Cr] UFGZSIPAQKLCGR-UHFFFAOYSA-N 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 4
- 229910001337 iron nitride Inorganic materials 0.000 claims description 4
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 4
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 claims description 4
- ZVWKZXLXHLZXLS-UHFFFAOYSA-N zirconium nitride Chemical compound [Zr]#N ZVWKZXLXHLZXLS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052580 B4C Inorganic materials 0.000 claims description 3
- 229910002601 GaN Inorganic materials 0.000 claims description 3
- CXOWYMLTGOFURZ-UHFFFAOYSA-N azanylidynechromium Chemical compound [Cr]#N CXOWYMLTGOFURZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052614 beryl Inorganic materials 0.000 claims description 3
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 229910003468 tantalcarbide Inorganic materials 0.000 claims description 3
- 229910052715 tantalum Inorganic materials 0.000 claims description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 3
- 229910052690 Einsteinium Inorganic materials 0.000 claims 1
- 238000013019 agitation Methods 0.000 claims 1
- 230000003746 surface roughness Effects 0.000 abstract description 16
- 230000003647 oxidation Effects 0.000 abstract description 11
- 238000007254 oxidation reaction Methods 0.000 abstract description 11
- 229910052691 Erbium Inorganic materials 0.000 abstract description 3
- 229910052689 Holmium Inorganic materials 0.000 abstract description 2
- 229910052706 scandium Inorganic materials 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 59
- 229910005335 FePt Inorganic materials 0.000 description 38
- 125000004429 atom Chemical group 0.000 description 19
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 17
- 239000002245 particle Substances 0.000 description 15
- 238000007731 hot pressing Methods 0.000 description 14
- 239000010410 layer Substances 0.000 description 14
- 238000002490 spark plasma sintering Methods 0.000 description 14
- 238000012360 testing method Methods 0.000 description 14
- 238000001513 hot isostatic pressing Methods 0.000 description 13
- 229910001260 Pt alloy Inorganic materials 0.000 description 9
- 239000003963 antioxidant agent Substances 0.000 description 9
- 230000003078 antioxidant effect Effects 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 8
- 230000003064 anti-oxidating effect Effects 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 238000003825 pressing Methods 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- TWFZGCMQGLPBSX-UHFFFAOYSA-N Carbendazim Natural products C1=CC=C2NC(NC(=O)OC)=NC2=C1 TWFZGCMQGLPBSX-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- MVXWAZXVYXTENN-UHFFFAOYSA-N azanylidyneuranium Chemical compound [U]#N MVXWAZXVYXTENN-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000006013 carbendazim Substances 0.000 description 2
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- 239000006249 magnetic particle Substances 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- DTJAVSFDAWLDHQ-UHFFFAOYSA-N [Cr].[Co].[Pt] Chemical compound [Cr].[Co].[Pt] DTJAVSFDAWLDHQ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- SJKRCWUQJZIWQB-UHFFFAOYSA-N azane;chromium Chemical compound N.[Cr] SJKRCWUQJZIWQB-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- JNPZQRQPIHJYNM-UHFFFAOYSA-N carbendazim Chemical compound C1=C[CH]C2=NC(NC(=O)OC)=NC2=C1 JNPZQRQPIHJYNM-UHFFFAOYSA-N 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
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- 230000007797 corrosion Effects 0.000 description 1
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- 230000001808 coupling effect Effects 0.000 description 1
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- 229910003460 diamond Inorganic materials 0.000 description 1
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- 239000007789 gas Substances 0.000 description 1
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- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
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- Manufacturing Of Magnetic Record Carriers (AREA)
Abstract
Description
本創作關於一種鐵鉑基靶材，尤指一種適用於磁記錄媒體之鐵鉑基靶材；此外，本創作另關於一種鐵鉑基靶材的製造方法。This invention relates to an iron-platinum-based target material, in particular to an iron-platinum-based target material suitable for magnetic recording media; in addition, this invention also relates to a method for manufacturing the iron-platinum-based target material.
磁記錄是指利用磁性材料的磁滯特性將資訊儲存於記錄媒體。根據磁頭磁化的方向，隨著消費者對可攜式記錄媒體的需求，以及大數據崛起、巨量資訊的產生，使得人們對於磁記錄媒體之資訊儲存容量的需求越來越大，因此，如何提升磁記錄媒體之記錄密度一直是相關領域關注的研究重點。Magnetic recording refers to the use of the hysteresis properties of magnetic materials to store information in recording media. According to the direction of the magnetization of the magnetic head, with the consumer's demand for portable recording media, the rise of big data, and the generation of massive amounts of information, people have an increasing demand for the information storage capacity of magnetic recording media. Therefore, how to improve the recording density of magnetic recording media has always been a research focus in related fields.
一般而言，垂直式磁記錄媒體的層狀結構由下至上包含有基板、附著層、軟磁層(soft underlayer)、晶種層(seed layer)、中間層(intermediate layer)、磁記錄層(magnetic recording layer)、潤滑層以及覆蓋層。隨著垂直式磁記錄媒體的技術趨於成熟，鈷鉻鉑基合金系統之磁記錄層亦逐漸接近磁記錄密度極限，為了再進一步提高垂直式磁記錄媒體的記錄密度，業界遂發展出選用鐵鉑基合金系統製作熱輔助磁記錄媒體(heat-assisted magnetic recording medium，HAMR medium)之磁記錄層，其係在寫入磁場的同時以熱能的方式作用於記錄位的磁性顆粒上，藉由將該磁性顆粒的溫度提高至居里點(Curie temperature)之上，使得該磁性顆粒的磁力頑性暫時被降低，又由於鐵鉑基合金的磁性顆粒尺寸可較鈷鉻鉑基合金的磁性顆粒尺寸縮小，進而可提高磁記錄媒體的記錄密度。此外，因熱輔助磁記錄的技術會在相同的區域重複聚焦加熱，需要以穩定性高的磁性複合材料作為磁記錄層，現有技術之熱輔助磁記錄層多半選用鐵鉑基合金系統作為磁記錄層的主要成分，並可於鐵鉑基合金系統中額外添加如氮化硼(boron nitride，BN)、碳等非磁性成分，藉此在鐵鉑基合金的晶粒之間形成阻隔及減少磁耦合效應。Generally speaking, the layered structure of a perpendicular magnetic recording medium includes a substrate, an adhesion layer, a soft underlayer, a seed layer, an intermediate layer, a magnetic recording layer, a lubricating layer, and a cover layer from bottom to top. As the technology of perpendicular magnetic recording media matures, the magnetic recording layer of the Cobalt-Chromium-Pt alloy system is gradually approaching the magnetic recording density limit. In order to further improve the recording density of perpendicular magnetic recording media, the industry has developed a heat-assisted magnetic recording medium (HAMR medium) made of an iron-platinum alloy system. The heat energy acts on the magnetic grains of the recording bit while writing the magnetic field, raising the temperature of the magnetic grains to the Curie point. temperature), the magnetic flexibility of the magnetic particles is temporarily reduced. Since the magnetic particle size of the iron-platinum alloy can be smaller than that of the cobalt-chromium-platinum alloy, the recording density of the magnetic recording medium can be increased. In addition, since the heat-assisted magnetic recording technology will repeatedly focus and heat the same area, a magnetic composite material with high stability is required as the magnetic recording layer. The heat-assisted magnetic recording layer of the existing technology mostly uses the iron-platinum alloy system as the main component of the magnetic recording layer, and non-magnetic components such as boron nitride (BN) and carbon can be added to the iron-platinum alloy system to form a barrier between the grains of the iron-platinum alloy and reduce the magnetic coupling effect.
然而，現有技術的鐵鉑基靶材存在相對密度不足和抗氧化能力差等問題。若鐵鉑基靶材不具備足夠的抗氧化能力，當未於適當條件下保存靶材時，靶材表面則很容易因發生氧化而產生鏽蝕的現象，影響磁記錄層的品質，嚴重影響後續進行濺鍍所製得之磁記錄層的應用。However, the existing FePt target has problems such as insufficient relative density and poor oxidation resistance. If the FePt target does not have sufficient oxidation resistance, when the target is not stored under appropriate conditions, the surface of the target will easily rust due to oxidation, affecting the quality of the magnetic recording layer and seriously affecting the application of the magnetic recording layer obtained by sputtering.
再者，隨著碟片記錄密度的提高及磁頭飛行高度的降低，亦須降低碟片上薄膜的表面粗糙度。Furthermore, as the recording density of the disc increases and the flying height of the magnetic head decreases, the surface roughness of the film on the disc must also be reduced.
有鑒於現有技術所面臨的缺陷，本創作之目的在於提升鐵鉑基靶材的抗氧化能力，使得本創作所提供之鐵鉑基靶材易於保存且能夠提高濺鍍形成的磁記錄層之品質與良率。In view of the defects faced by the existing technology, the purpose of this invention is to enhance the anti-oxidation ability of the FePt-based target material, so that the FePt-based target material provided by this invention is easy to preserve and can improve the quality and yield of the magnetic recording layer formed by sputtering.
本創作之另一目的在於提供一種鐵鉑基靶材，利用所述鐵鉑基靶材濺鍍形成的鐵鉑基薄膜具有較低的表面粗糙度。Another object of the present invention is to provide an iron-platinum-based target material, wherein an iron-platinum-based film formed by sputtering using the iron-platinum-based target material has a lower surface roughness.
為達成前述目的，本創作提供一種鐵鉑基靶材，其包含鐵(Iron，Fe)、鉑(Platinum，Pt)、第一成分以及氮化物(nitride)；其中該第一成分係選自釕(Ruthenium，Ru)、錳(Manganese，Mn)、硼(Boron，B)、銠(Rhodium，Rh)、銥(Iridium，Ir)、鈮(Niobium，Nb)、鈧(Scandium，Sc)、釔(Yttrium，Y)、鈥(Holmium，Ho)、鉺(Erbium，Er)、釩(Vanadium，V)、鋯(Zirconium，Zr)及其組合所組成之群組；其中，以該鐵鉑基靶材整體之原子總數為基準，該第一成分的含量係大於或等於2原子百分比(atomic percentage，at%)且小於或等於12 at%，該氮化物的含量係大於或等於8 at%且小於或等於30 at%；該鐵鉑基靶材中的鈣(Calcium，Ca)含量係小於百萬分之20 (即，20 parts per million，20 ppm)，以及該鐵鉑基靶材中的氧(Oxygen，O)含量係小於1000 ppm；其中，該鐵鉑基靶材的相對密度係大於98%。To achieve the above-mentioned purpose, the present invention provides an iron-platinum-based target material, which comprises iron (Fe), platinum (Pt), a first component and a nitride; wherein the first component is selected from the group consisting of ruthenium (Ru), manganese (Mn), boron (B), rhodium (Rh), iridium (Ir), niobium (Nb), scandium (Sc), yttrium (Y), holmium (Ho), erbium (Er), vanadium (V), zirconium (Zr) and combinations thereof; wherein, based on the total number of atoms in the entire iron-platinum-based target material, the content of the first component is greater than or equal to 2 atomic percentage (atomic percentage, at%) and less than or equal to 12 at%, the content of the nitride is greater than or equal to 8 at% and less than or equal to 30 at%; the content of calcium (Ca) in the FePt-based target is less than 20 parts per million (ppm), and the content of oxygen (O) in the FePt-based target is less than 1000 ppm; wherein the relative density of the FePt-based target is greater than 98%.
藉由控制本創作之鐵鉑基靶材同時兼具以下技術特徵：(I)所述第一成分含量大於或等於2 at%且小於或等於12 at%、(II)所述氮化物含量大於或等於8 at%且小於或等於30 at%、(III)鐵鉑基靶材中的鈣含量小於20 ppm、(IV)鐵鉑基靶材中的氧含量小於1000 ppm以及(Ⅴ)鐵鉑基靶材的相對密度大於98%，能有效提升鐵鉑基靶材的抗氧化能力；此外，由所述鐵鉑基靶材濺鍍形成的鐵鉑基薄膜還可具有足夠小的表面粗糙度。By controlling the content of the first component in the iron-platinum-based target of the present invention to have the following technical characteristics at the same time: (I) the content of the first component is greater than or equal to 2 at% and less than or equal to 12 at%, (II) the content of the nitride is greater than or equal to 8 at% and less than or equal to 30 at%, (III) the calcium content in the iron-platinum-based target is less than 20 ppm, (IV) the oxygen content in the iron-platinum-based target is less than 1000 ppm, and (V) the relative density of the iron-platinum-based target is greater than 98%, the oxidation resistance of the iron-platinum-based target can be effectively improved; in addition, the iron-platinum-based film formed by sputtering of the iron-platinum-based target can also have a sufficiently small surface roughness.
較佳的，以整體鐵鉑基靶材之原子總數為基準，鐵的含量係大於或等於8 at%且小於或等於77 at%，但不限於此。更佳的，以該鐵鉑基靶材整體之原子總數為基準，鐵的含量係大於或等於34 at%且小於或等於75 at%。Preferably, based on the total number of atoms in the entire FePt-based target, the content of iron is greater than or equal to 8 at% and less than or equal to 77 at%, but not limited thereto. More preferably, based on the total number of atoms in the entire FePt-based target, the content of iron is greater than or equal to 34 at% and less than or equal to 75 at%.
較佳的，以整體鐵鉑基靶材之原子總數為基準，鉑的含量係大於或等於3 at%且小於或等於30 at%，但不限於此。Preferably, based on the total number of atoms in the entire FePt-based target, the content of platinum is greater than or equal to 3 at% and less than or equal to 30 at%, but is not limited thereto.
較佳的，該氮化物係選自氮化硼(BN)、氮化鋁(AlN)、氮化釩(VN)、氮化鈧(ScN)、氮化錳(MnN)、氮化鈦(TiN)、氮化鐵(FeN)、氮化鎵(GaN)、氮化鎳(NiN)、氮化鋯(ZrN)、氮化鈮(NbN)、氮化矽(Si 3N 4)、氮化鉿(HfN)、氮化鉭(TaN)、氮化鉬(MoN)、氮化鈷(CoN)、氮化鉻(CrN)及其組合所組成之群組。依據本創作，當氮化物只有一種選擇時，則所述「氮化物的含量」即是該單一種氮化物的含量；當氮化物包含有二種以上選擇時，所述「氮化物的含量」即是該些氮化物之個別含量的總和；舉例而言，當氮化物為7 at%的氮化硼、10 at%的氮化錳和10 at%的氮化鈦之組合時，則氮化物的含量即為27 at%。 Preferably, the nitride is selected from the group consisting of boron nitride (BN), aluminum nitride (AlN), vanadium nitride (VN), sintered carbide nitride (ScN), manganese nitride (MnN), titanium nitride (TiN), iron nitride (FeN), gallium nitride (GaN), nickel nitride (NiN), zirconium nitride (ZrN), niobium nitride (NbN), silicon nitride (Si 3 N 4 ), helium nitride (HfN), tantalum nitride (TaN), molybdenum nitride (MoN), cobalt nitride (CoN), chromium nitride (CrN) and combinations thereof. According to the present invention, when there is only one choice of nitride, the "nitride content" is the content of the single nitride; when the nitride includes two or more choices, the "nitride content" is the sum of the individual contents of these nitrides; for example, when the nitride is a combination of 7 at% boron nitride, 10 at% manganese nitride and 10 at% titanium nitride, the nitride content is 27 at%.
較佳的，該鐵鉑基靶材中的鈣含量係為1 ppm至11 ppm，但不限於此。Preferably, the calcium content in the FePt-based target is 1 ppm to 11 ppm, but not limited thereto.
較佳的，當該鐵鉑基靶材中的氧含量係小於625 ppm，可更進一步提升其抗氧化能力。更佳的，該鐵鉑基靶材中的氧含量係小於510 ppm。Preferably, when the oxygen content in the FePt-based target is less than 625 ppm, its anti-oxidation ability can be further improved. More preferably, the oxygen content in the FePt-based target is less than 510 ppm.
在一些實施態樣中，該鐵鉑基靶材更包含碳(C)或碳化物。具體而言，該碳化物係選自碳化鎢(WC)、碳化鈦(TiC)、碳化鈮(NbC)、碳化鉭(TaC X，X=0.4至1)、碳化鉻(Cr 3C 2)、碳化矽(SiC)、碳化鋯(ZrC)、碳化硼(B 4C)、碳化釩(VC)、碳化鉿(HfC)、氮碳化鈦(TiCN)及其組合所組成之群組。 In some embodiments, the iron platinum-based target further comprises carbon (C) or carbide. Specifically, the carbide is selected from the group consisting of tungsten carbide (WC), titanium carbide (TiC), niobium carbide (NbC), tantalum carbide ( TaCX , X=0.4 to 1), chromium carbide ( Cr3C2 ), silicon carbide ( SiC ), zirconium carbide (ZrC), boron carbide ( B4C ), vanadium carbide (VC), niobium carbide (HfC), titanium carbide nitrogen (TiCN) and combinations thereof.
具體而言，該鐵鉑基靶材中碳的型態可為具有三維四面體結構的鑽石碳、二維平面結構的石墨碳、一維結構的奈米碳管，或其組合，但不限於此。Specifically, the carbon in the iron platinum-based target can be in the form of diamond carbon with a three-dimensional tetrahedral structure, graphite carbon with a two-dimensional planar structure, carbon nanotubes with a one-dimensional structure, or a combination thereof, but is not limited thereto.
較佳的，以該鐵鉑基靶材整體之原子總數為基準，該碳和碳化物的總含量係大於或等於10 at%且小於或等於20 at%，其中，碳之含量可為0 at%，或者碳化物之含量可為0 at%，但不限於此。類似地，依據本創作，當碳或碳化物只有一種選擇時，則所述「碳和碳化物的總含量」即是該單一種選擇的含量；當碳和碳化物包含有二種以上選擇時，所述「碳和碳化物的總含量」即是該些選擇之個別含量的總和；舉例而言，當碳或碳化物為6 at%的碳和10 at%的碳化鈮之組合時，則碳和碳化物的總含量即為16 at%。Preferably, based on the total number of atoms of the entire iron-platinum-based target material, the total content of carbon and carbide is greater than or equal to 10 at% and less than or equal to 20 at%, wherein the carbon content may be 0 at%, or the carbide content may be 0 at%, but is not limited thereto. Similarly, according to the present invention, when there is only one option for carbon or carbide, the "total content of carbon and carbide" is the content of the single option; when carbon and carbide include more than two options, the "total content of carbon and carbide" is the sum of the individual contents of these options; for example, when carbon or carbide is a combination of 6 at% carbon and 10 at% niobium carbide, the total content of carbon and carbide is 16 at%.
依據本創作，該鐵鉑基靶材的相對密度係大於98%。較佳的，該鐵鉑基靶材的相對密度係大於98.2%，但不限於此。更佳的，該鐵鉑基靶材的相對密度係大於99%，但不限於此。其中，前述相對密度係採用阿基米德法(Archimedes principle)量測所得。According to the present invention, the relative density of the iron-platinum-based target is greater than 98%. Preferably, the relative density of the iron-platinum-based target is greater than 98.2%, but not limited thereto. More preferably, the relative density of the iron-platinum-based target is greater than 99%, but not limited thereto. The relative density is measured using the Archimedes principle.
此外，本創作另提供一種鐵鉑基靶材的製造方法，其包含以下步驟：步驟(a)：將鐵原料、鉑原料、第一成分原料以及氮化物原料混合再研磨，得到一原料混合物；其中，該第一成分係選自釕、錳、硼、銠、銥、鈮、鈧、釔、鈥、鉺、釩、鋯及其組合所組成之群組；以該原料混合物整體之原子總數為基準，該第一成分原料的添加量係大於或等於2 at%且小於或等於12 at%，該氮化物原料的添加量係大於或等於8 at%且小於或等於30 at%；；步驟(b)：將該原料混合物置於一水中進行攪拌水洗工序，得到一水洗後的原料混合物；其中，該水的溫度係大於或等於55℃且小於或等於65℃；步驟(c)：將該水洗後的原料混合物進行乾燥處理工序，得到一乾燥後的原料混合物；步驟(d)：將該乾燥後的原料混合物進行氫氣還原工序，得到一還原材料；以及步驟(e)：燒結該還原材料，獲得該鐵鉑基靶材；其中，該鐵鉑基靶材中的鈣含量係小於20 ppm，以及該鐵鉑基靶材中的氧含量係小於1000 ppm；該鐵鉑基靶材的相對密度係大於98%。In addition, the invention further provides a method for manufacturing an iron-platinum-based target, which comprises the following steps: step (a): mixing an iron raw material, a platinum raw material, a first component raw material and a nitride raw material and grinding them to obtain a raw material mixture; wherein the first component is selected from the group consisting of ruthenium, manganese, boron, rhodium, iridium, niobium, arsenic, yttrium, tantalum, beryl, vanadium, zirconium and combinations thereof; based on the total number of atoms in the raw material mixture as a whole, the addition amount of the first component raw material is greater than or equal to 2 at% and less than or equal to 12 at%, and the addition amount of the nitride raw material is greater than or equal to 8 at% and less than or equal to 30 at%. at%; step (b): placing the raw material mixture in water for a stirring and washing process to obtain a washed raw material mixture; wherein the temperature of the water is greater than or equal to 55°C and less than or equal to 65°C; step (c): performing a drying process on the washed raw material mixture to obtain a dried raw material mixture; step (d): performing a hydrogen reduction process on the dried raw material mixture to obtain a reduced material; and step (e): sintering the reduced material to obtain the iron-platinum-based target material; wherein the calcium content in the iron-platinum-based target material is less than 20 ppm, and the oxygen content in the iron-platinum-based target material is less than 1000 ppm; the relative density of the iron-platinum-based target material is greater than 98%.
本創作藉由限定第一成分原料與氮化物原料的使用量範圍，以及透過水洗、乾燥工序降低原料混合物中所含的鈣含量，並將所有原料混合物再進行氫氣還原工序，有助於控制鐵鉑基靶材的氧含量，因此，後續形成鐵鉑基靶材時，還可具有大於98%的相對密度，進而提升該鐵鉑基靶材的抗氧化能力，並且，利用所述鐵鉑基靶材濺鍍形成的鐵鉑基薄膜具有較低的表面粗糙度。This invention helps to control the oxygen content of the iron-platinum-based target by limiting the usage range of the first component raw material and the nitride raw material, reducing the calcium content in the raw material mixture through water washing and drying processes, and subjecting all the raw material mixtures to a hydrogen reduction process. Therefore, when the iron-platinum-based target is subsequently formed, it can also have a relative density greater than 98%, thereby improving the oxidation resistance of the iron-platinum-based target. In addition, the iron-platinum-based film formed by sputtering using the iron-platinum-based target has a lower surface roughness.
依據本創作，該步驟(a)中，鐵原料可為純度為99%以上的鐵金屬、鐵含量為50重量百分比(wt%)以上的鐵合金、或其組合，但並非僅限於此。較佳的，該鐵原料的平均粒徑為5微米(μm)至80 μm。According to the present invention, in step (a), the iron raw material can be an iron metal with a purity of more than 99%, an iron alloy with an iron content of more than 50 weight percent (wt%), or a combination thereof, but is not limited thereto. Preferably, the average particle size of the iron raw material is 5 micrometers (μm) to 80 μm.
依據本創作，該步驟(B)中，鉑原料可為純度為99%以上的鉑金屬、鉑含量為50 wt%以上的鉑合金、或其組合，但並非僅限於此。較佳的，該鉑原料的平均粒徑為1 μm至10 μm，但不限於此。藉由選擇平均粒徑為前述範圍的鉑原料，可使鉑較容易在鐵相中擴散。According to the present invention, in step (B), the platinum raw material can be a platinum metal with a purity of 99% or more, a platinum alloy with a platinum content of 50 wt% or more, or a combination thereof, but is not limited thereto. Preferably, the average particle size of the platinum raw material is 1 μm to 10 μm, but is not limited thereto. By selecting a platinum raw material with an average particle size in the aforementioned range, platinum can be more easily diffused in the iron phase.
在一些實施例中，鉑原料和鐵原料可為鐵鉑合金。In some embodiments, the platinum raw material and the iron raw material may be an iron-platinum alloy.
較佳的，該第一成分原料的平均粒徑5 μm至50 μm，但不限於此。Preferably, the average particle size of the first component raw material is 5 μm to 50 μm, but not limited thereto.
較佳的，該氮化物原料的平均粒徑0.1 μm至30 μm，但不限於此。Preferably, the average particle size of the nitride raw material is 0.1 μm to 30 μm, but not limited thereto.
具體而言，該氮化物原料可選自氮化硼原料、氮化鋁原料、氮化釩原料、氮化鈧原料、氮化錳原料、氮化鈦原料、氮化鐵原料、氮化鎵原料、氮化鎳原料、氮化鋯原料、氮化鈮原料、氮化矽原料、氮化鉿原料、氮化鉭原料、氮化鉬原料、氮化鈷原料、氮化鉻原料及其組合所組成之群組。Specifically, the nitride raw material can be selected from the group consisting of boron nitride raw materials, aluminum nitride raw materials, vanadium nitride raw materials, carbendazim raw materials, manganese nitride raw materials, titanium nitride raw materials, iron nitride raw materials, gallium nitride raw materials, nickel nitride raw materials, zirconium nitride raw materials, niobium nitride raw materials, silicon nitride raw materials, uranium nitride raw materials, tantalum nitride raw materials, molybdenum nitride raw materials, cobalt nitride raw materials, chromium nitride raw materials and combinations thereof.
在一些實施例中，該步驟(a)中更包括碳原料或碳化物原料。較佳的，該碳原料或碳化物原料的平均粒徑0.1 μm至30 μm，但不限於此。In some embodiments, the step (a) further comprises a carbon raw material or a carbide raw material. Preferably, the carbon raw material or the carbide raw material has an average particle size of 0.1 μm to 30 μm, but is not limited thereto.
具體而言，該碳化物原料可選自碳化鎢原料、碳化鈦原料、碳化鈮原料、碳化鉭原料、碳化鉻原料、碳化矽原料、碳化鋯原料、碳化硼原料、碳化釩原料、碳化鉿原料、氮碳化鈦原料及其組合所組成之群組。Specifically, the carbide raw material can be selected from the group consisting of tungsten carbide raw materials, titanium carbide raw materials, niobium carbide raw materials, tungsten carbide raw materials, chromium carbide raw materials, silicon carbide raw materials, zirconium carbide raw materials, boron carbide raw materials, vanadium carbide raw materials, niobium carbide raw materials, titanium carbide nitrogen raw materials and combinations thereof.
依據本創作，在該步驟(a)中，該混合方式可選用任何能夠均勻混合原料的方式。此外，該步驟(a)中，可使用一高速研磨機進行該研磨工序，但不限於此。較佳的，該步驟(a)中的研磨時間為1小時至4小時，但不限於此。According to the invention, in step (a), the mixing method can be any method that can evenly mix the raw materials. In addition, in step (a), a high-speed grinder can be used to perform the grinding process, but it is not limited thereto. Preferably, the grinding time in step (a) is 1 hour to 4 hours, but it is not limited thereto.
較佳的，於該步驟(b)中，該原料混合物的重量與該水的體積之比值為大於或等於90克/公升(g/L)且小於或等於110g/L，例如，95 g/L、98 g/L、100 g/L、105 g/L、108 g/L，但不限於此。Preferably, in step (b), the ratio of the weight of the raw material mixture to the volume of the water is greater than or equal to 90 g/L and less than or equal to 110 g/L, for example, 95 g/L, 98 g/L, 100 g/L, 105 g/L, 108 g/L, but not limited thereto.
較佳的，於該步驟(c)中，該乾燥處理工序的持續時間係大於或等於6小時且小於或等於18小時，但不限於此。較佳的，於該步驟(c)中，該乾燥處理工序的溫度係大於或等於70℃且小於或等於90℃，例如，75℃、80℃、85℃，但不限於此。本創作藉由水洗工序降低該原料混合物中的鈣含量，因此，最後所得之鐵鉑基靶材的鈣含量即大致等同於乾燥後的原料混合物中的鈣含量。Preferably, in step (c), the duration of the drying process is greater than or equal to 6 hours and less than or equal to 18 hours, but not limited thereto. Preferably, in step (c), the temperature of the drying process is greater than or equal to 70°C and less than or equal to 90°C, for example, 75°C, 80°C, 85°C, but not limited thereto. The present invention reduces the calcium content in the raw material mixture by a water washing process, so the calcium content of the iron platinum-based target material obtained in the end is roughly equivalent to the calcium content in the raw material mixture after drying.
較佳的，於該步驟(d)中，該氫氣還原工序的持續時間係大於或等於1小時且小於或等於3小時，但不限於此；還原溫度係大於或等於550℃且小於或等於900℃，但不限於此。具體而言，於該步驟(d)中，該乾燥後的原料混合物係置於氫氣氣氛環境、溫度為550℃至900℃之條件下進行熱處理1小時至3小時，以獲得所述還原材料，但不限於此。Preferably, in the step (d), the duration of the hydrogen reduction process is greater than or equal to 1 hour and less than or equal to 3 hours, but not limited thereto; the reduction temperature is greater than or equal to 550° C. and less than or equal to 900° C., but not limited thereto. Specifically, in the step (d), the dried raw material mixture is placed in a hydrogen atmosphere at a temperature of 550° C. to 900° C. for 1 hour to 3 hours to obtain the reduced material, but not limited thereto.
在一些實施態樣中，該步驟(d)和該步驟(e)中可更包括一預壓步驟；即於該步驟(d)中獲得所述還原材料後，可接續進行一預壓步驟，該預壓步驟可為任何能夠將所述還原材料壓製成為具有固定形狀的手段。舉例而言，該預壓步驟可為將所述還原材料置入油壓機中並以約為15巴(bar)至110 bar之壓力進行預壓，但不限於此。In some embodiments, the step (d) and the step (e) may further include a pre-pressing step; that is, after obtaining the reduced material in the step (d), a pre-pressing step may be performed successively, and the pre-pressing step may be any means capable of pressing the reduced material into a fixed shape. For example, the pre-pressing step may be placing the reduced material in a hydraulic press and pre-pressing it at a pressure of about 15 bar to 110 bar, but is not limited thereto.
依據本創作，於該步驟(e)中，所述燒結的方式可單獨採用熱壓成型法(hot pressing，HP)、熱均壓成型法(hot isostatic pressing，HIP)或放電等離子體燒結法(spark plasma sintering，SPS)，亦可結合前述燒結方式之兩者以上進行燒結。較佳的，於該步驟(e)中，燒結溫度可以係大於或等於700℃且小於或等於1200℃，燒結壓力可以係大於或等於220 bar且小於或等於1850 bar。舉例而言，當採用HP進行燒結時，其燒結溫度可為800°C至1200°C，燒結壓力可為350 bar至400 bar，燒結時間可為1小時至4小時，但不限於此；當採用HIP進行燒結時，其燒結溫度可為800°C至1200°C，燒結壓力可為1200 bar至1850 bar，燒結時間可為1小時至4小時，但不限於此；當採用SPS進行燒結時，其燒結溫度可為700°C至1200°C，燒結壓力可為220 bar至1200 bar，燒結時間可為5分鐘至2小時，但不限於此。According to the present invention, in step (e), the sintering method may be hot pressing (HP), hot isostatic pressing (HIP) or spark plasma sintering (SPS), or two or more of the above sintering methods may be combined for sintering. Preferably, in step (e), the sintering temperature may be greater than or equal to 700°C and less than or equal to 1200°C, and the sintering pressure may be greater than or equal to 220 bar and less than or equal to 1850 bar. For example, when HP is used for sintering, the sintering temperature may be 800°C to 1200°C, the sintering pressure may be 350 bar to 400 bar, and the sintering time may be 1 hour to 4 hours, but not limited thereto; when HIP is used for sintering, the sintering temperature may be 800°C to 1200°C, the sintering pressure may be 1200 bar to 1850 bar, and the sintering time may be 1 hour to 4 hours, but not limited thereto; when SPS is used for sintering, the sintering temperature may be 700°C to 1200°C, the sintering pressure may be 220 bar to 1200 bar, and the sintering time may be 5 minutes to 2 hours, but not limited thereto.
於本說明書中，由「小數值至大數值」表示的範圍，如果沒有特別指明，則表示其範圍為大於或等於該小數值且小於或等於該大數值。例如：研磨時間為1小時至4小時，即表示研磨時間範圍為「大於或等於1小時且小於或等於4小時」。In this manual, if there is no special indication, the range expressed by "a small number to a large number" means that the range is greater than or equal to the small number and less than or equal to the large number. For example, if the grinding time is 1 hour to 4 hours, it means that the grinding time range is "greater than or equal to 1 hour and less than or equal to 4 hours".
為驗證鐵鉑基靶材中的材料組成、製備方法中的水洗、氫氣還原等工序對鐵鉑基靶材的影響，以下列舉數種鐵鉑基靶材作為例示，詳細說明本創作的實施方式，所屬技術領域具有通常知識者可經由本說明書之內容輕易地了解本創作所能達成之優點與功效，並且於不悖離本創作之精神下進行各種修飾與變更，以施行或應用本創作之內容。In order to verify the material composition of the iron-platinum-based target, the influence of water washing, hydrogen reduction and other processes in the preparation method on the iron-platinum-based target, several iron-platinum-based targets are listed below as examples to explain in detail the implementation method of the present invention. A person with ordinary knowledge in the relevant technical field can easily understand the advantages and effects that can be achieved by the present invention through the contents of this manual, and make various modifications and changes without deviating from the spirit of the present invention to implement or apply the contents of the present invention.
實施例Embodiment 11 至to 14 (E1-E14)14 (E1-E14) ：鐵鉑基靶材：FePt based target
首先，依據表1-1所列之鐵鉑基靶材的組成，秤取適量平均粒徑為10 μm之鐵粉末、平均粒徑為5 μm之鉑粉末、平均粒徑為15 μm之第一成分粉末以及平均粒徑為5 μm之氮化物粉末置於高速研磨機中進行混合，隨後再進行研磨1至4小時，得到一原料混合物。First, according to the composition of the iron-platinum-based target listed in Table 1-1, appropriate amounts of iron powder with an average particle size of 10 μm, platinum powder with an average particle size of 5 μm, first component powder with an average particle size of 15 μm, and nitride powder with an average particle size of 5 μm are weighed and mixed in a high-speed grinder, and then ground for 1 to 4 hours to obtain a raw material mixture.
其次，將前述原料混合物置於溫度為60℃的水中，進行攪拌水洗工序3小時，得到一水洗後的原料混合物；其中，前述原料混合物的重量與水的體積之比值為100 g/1L。接著，將水洗後的原料混合物置於一溫度設定於80℃的烘箱中持續乾燥12小時，得到一乾燥後的原料混合物，此時，所述乾燥後的原料混合物的鈣含量小於20 ppm。Secondly, the raw material mixture is placed in water at a temperature of 60°C and stirred and washed for 3 hours to obtain a washed raw material mixture; wherein the ratio of the weight of the raw material mixture to the volume of water is 100 g/1L. Then, the washed raw material mixture is placed in an oven set at a temperature of 80°C and dried for 12 hours to obtain a dried raw material mixture, at which time, the calcium content of the dried raw material mixture is less than 20 ppm.
然後，將前述乾燥後的原料混合物置於750℃的氫氣氣氛中進行還原1小時，得到一還原材料。Then, the dried raw material mixture is placed in a hydrogen atmosphere at 750° C. for reduction for 1 hour to obtain a reduced material.
接著，將該還原材料置入油壓機中並以約為20 bar之壓力進行預壓，隨後依據表1-2所列之燒結製程以及燒結溫度進行燒結，以獲得實施例1至14之鐵鉑基靶材；其中，若採用HP進行燒結，其燒結壓力約為380 bar、燒結時間為3小時；若採用HIP進行燒結，其燒結壓力約為1750 bar、燒結時間為3小時；若採用SPS進行燒結，其燒結壓力約為252 bar、燒結時間為10分鐘。Next, the reduced material is placed in a hydraulic press and pre-pressed at a pressure of about 20 bar, and then sintered according to the sintering process and sintering temperature listed in Table 1-2 to obtain the iron-platinum-based target materials of Examples 1 to 14; wherein, if HP is used for sintering, the sintering pressure is about 380 bar and the sintering time is 3 hours; if HIP is used for sintering, the sintering pressure is about 1750 bar and the sintering time is 3 hours; if SPS is used for sintering, the sintering pressure is about 252 bar and the sintering time is 10 minutes.
於表1-1中，實施例1至14之鐵鉑基靶材的組成可由aFe-bPt-cX-dY之通式所示，且各鐵鉑基靶材中的氧含量係小於1000 ppm；其中，a代表鐵原子數相對於鐵鉑基靶材之原子總數的含量比例；b代表鉑原子數相對於鐵鉑基靶材之原子總數的含量比例；c代表第一成分的原子數相對於鐵鉑基靶材之原子總數的含量比例，X代表第一成分，其可選自釕、錳、硼、銠、銥、鈮、鈧、釔、鈥、鉺、釩、鋯及其組合所組成之群組；d代表氮化物的原子數相對於鐵鉑基靶材之原子總數的含量比例，Y代表氮化物，其係選自氮化硼、氮化鋁、氮化釩、氮化鈧、氮化錳、氮化鈦、氮化鐵、氮化鎵、氮化鎳、氮化鋯、氮化鈮、氮化矽、氮化鉿、氮化鉭、氮化鉬、氮化鈷、氮化鉻及其組合所組成之群組。以氮化物為氮化硼時為例，d代表氮原子數及硼原子數的總和相對於鐵鉑基靶材之原子總數的含量比例。In Table 1-1, the composition of the FePt-based target of Examples 1 to 14 can be represented by the general formula of aFe-bPt-cX-dY, and the oxygen content in each FePt-based target is less than 1000 ppm; wherein a represents the content ratio of the number of iron atoms relative to the total number of atoms of the FePt-based target; b represents the content ratio of the number of platinum atoms relative to the total number of atoms of the FePt-based target; c represents the content ratio of the number of atoms of the first component relative to the total number of atoms of the FePt-based target, and X represents the first component, which can be selected from ruthenium, manganese, boron, rhodium, iridium, niobium, arsenic, yttrium, tantalum, erbium, vanadium, zirconium and the like. The target material is a group of a plurality of materials, wherein d represents the content ratio of the number of atoms of the nitride relative to the total number of atoms of the Fe-Pb-based target material, and Y represents a nitride selected from the group consisting of boron nitride, aluminum nitride, vanadium nitride, carbendazim nitride, manganese nitride, titanium nitride, iron nitride, gallium nitride, nickel nitride, zirconium nitride, niobium nitride, silicon nitride, uranium nitride, tantalum nitride, molybdenum nitride, cobalt nitride, chromium nitride, and combinations thereof. For example, when the nitride is boron nitride, d represents the content ratio of the sum of the number of nitrogen atoms and the number of boron atoms relative to the total number of atoms of the Fe-Pb-based target material.
其中，以實施例1之鐵鉑基靶材為例，相對於鐵鉑基靶材之原子總數，Fe佔46 at%；Pt佔25 at%；第一成分為Ru和B，且Ru佔4 at%、B佔1 at%，因此，第一成分共佔5 at%；以及氮化物為AlN，其佔24 at%。另外，以實施例2之鐵鉑基靶材為例，相對於鐵鉑基靶材之原子總數，Fe佔62 at%；Pt佔13 at%；第一成分為V和Zr，且V佔4 at%、Zr佔4 at%，因此，第一成分共佔8 at%；以及氮化物為ScN和VN，且ScN佔7 at%、VN佔10 at%，因此，氮化物共佔17 at%。Among them, taking the iron platinum-based target of Example 1 as an example, relative to the total number of atoms of the iron platinum-based target, Fe accounts for 46 at%, Pt accounts for 25 at%, the first component is Ru and B, and Ru accounts for 4 at%, B accounts for 1 at%, so the first component accounts for 5 at% in total; and the nitride is AlN, which accounts for 24 at%. In addition, taking the iron platinum-based target of Example 2 as an example, relative to the total number of atoms of the iron platinum-based target, Fe accounts for 62 at%, Pt accounts for 13 at%, the first component is V and Zr, and V accounts for 4 at%, Zr accounts for 4 at%, so the first component accounts for 8 at% in total; and the nitride is ScN and VN, and ScN accounts for 7 at%, VN accounts for 10 at%, so the nitride accounts for 17 at%.
實施例Embodiment 1515 至to 20 (E15-E20)20 (E15-E20) ：: 鐵鉑基靶材Iron platinum based target (( 含有碳Contains carbon ))
實施例15至20與實施例1至14的製作流程相似，即秤取適量的不同成分粉末經過混合、研磨、水洗、乾燥、氫氣還原、預壓以及燒結等步驟後，獲得實施例15至20之鐵鉑基靶材。The manufacturing process of Examples 15 to 20 is similar to that of Examples 1 to 14, that is, appropriate amounts of powders of different components are weighed and mixed, ground, washed, dried, hydrogen reduced, pre-pressed, and sintered to obtain the iron-platinum-based targets of Examples 15 to 20.
實施例15至20與實施例1至14主要差異在於，增加了碳和/或碳化物之成分。即依據表1-1所列之鐵鉑基靶材的組成，秤取適量平均粒徑為10 μm之鐵粉末、平均粒徑為5 μm之鉑粉末、平均粒徑為15 μm之第一成分粉末、平均粒徑5μm之氮化物粉末以及平均粒徑為3 μm之碳粉末或碳化物粉末置於高速研磨機中進行混合。The main difference between Examples 15 to 20 and Examples 1 to 14 is that carbon and/or carbide components are added. That is, according to the composition of the iron-platinum-based target material listed in Table 1-1, appropriate amounts of iron powder with an average particle size of 10 μm, platinum powder with an average particle size of 5 μm, first component powder with an average particle size of 15 μm, nitride powder with an average particle size of 5 μm, and carbon powder or carbide powder with an average particle size of 3 μm are weighed and placed in a high-speed grinder for mixing.
於表1-1中，實施例15至20之鐵鉑基靶材的組成可由aFe-bPt-cX-dY-eZ之通式所示；其中，a、b、c、X、d、Y如前述分別代表鐵原子數相對於鐵鉑基靶材之原子總數的含量比例、鉑原子數相對於鐵鉑基靶材之原子總數的含量比例、第一成分的選擇及其的原子數相對於鐵鉑基靶材之原子總數的含量比例，氮化物的選擇及其的原子數相對於鐵鉑基靶材之原子總數的含量比例，以及Z代表碳和/或碳化物的選擇，碳化物可選自碳化鎢、碳化鈦、碳化鈮、碳化鉭、碳化鉻、碳化矽、碳化鋯、碳化硼、碳化釩、碳化鉿、氮碳化鈦及其組合所組成之群組，e則代表碳和/或碳化物的原子數相對於鐵鉑基靶材之原子總數的含量比例。In Table 1-1, the composition of the Fe-Pt-based target of Examples 15 to 20 can be represented by the general formula of aFe-bPt-cX-dY-eZ; wherein a, b, c, X, d, and Y respectively represent the content ratio of the number of iron atoms relative to the total number of atoms of the Fe-Pt-based target, the content ratio of the number of platinum atoms relative to the total number of atoms of the Fe-Pt-based target, the selection of the first component and the content of its atomic number relative to the total number of atoms of the Fe-Pt-based target as described above. The ratio of nitride and the content ratio of its atomic number relative to the total atomic number of the iron-platinum-based target, and Z represents the selection of carbon and/or carbide, the carbide can be selected from the group consisting of tungsten carbide, titanium carbide, niobium carbide, tantalum carbide, chromium carbide, silicon carbide, zirconium carbide, boron carbide, vanadium carbide, arsenic carbide, titanium carbide nitride and combinations thereof, and e represents the content ratio of carbon and/or carbide atoms relative to the total atomic number of the iron-platinum-based target.
比較例Comparison Example 1 (C1)1 (C1) ：鐵鉑基靶材：FePt based target
比較例1之鐵鉑基靶材所採用的方法與實施例1之鐵鉑基靶材的製備方法大致相同，其主要差異在於：比較例1未經過水洗、乾燥、和氫氣還原之步驟，且燒結溫度略有差異。即依據表1-1所列之鐵鉑基靶材的組成秤取各原料之粉末，經過混合、研磨、預壓以及燒結等步驟後，製得比較例1之鐵鉑基靶材。比較例1的燒結製程以及燒結溫度列於表1-2中。The method used for preparing the iron platinum-based target material of Comparative Example 1 is substantially the same as the method for preparing the iron platinum-based target material of Example 1, and the main differences are: Comparative Example 1 does not undergo the steps of water washing, drying, and hydrogen reduction, and the sintering temperature is slightly different. That is, according to the composition of the iron platinum-based target material listed in Table 1-1, the powders of each raw material are weighed, and after the steps of mixing, grinding, pre-pressing, and sintering, the iron platinum-based target material of Comparative Example 1 is prepared. The sintering process and sintering temperature of Comparative Example 1 are listed in Table 1-2.
比較例Comparison Example 22 至to 5 (C2-C5)5 (C2-C5) ：鐵鉑基靶材：FePt based target
比較例2至5之鐵鉑基靶材所採用的方法與實施例1至14之鐵鉑基靶材的製備方法大致相同，其主要差異在於：比較例2未同時控制原料混合物中第一成分原料和氮化物原料之含量，以及未控制鐵鉑基靶材中的鈣含量；比較例3未控制原料混合物中第一成分原料之含量，以及未控制鐵鉑基靶材中的氧含量；比較例4、5皆未控制原料混合物中氮化物原料含量，未經過水洗、乾燥、和氫氣還原之步驟，以及未控制鐵鉑基靶材中的氧含量和鈣含量。比較例2至5之鐵鉑基靶材的組成、鈣含量和氧含量皆列於表1-1中，而燒結製程以及燒結溫度則列於表1-2中。The methods used for preparing the iron-platinum-based targets of Comparative Examples 2 to 5 are substantially the same as the methods for preparing the iron-platinum-based targets of Examples 1 to 14, with the main differences being that: Comparative Example 2 does not simultaneously control the contents of the first component raw material and the nitride raw material in the raw material mixture, and does not control the calcium content in the iron-platinum-based target; Comparative Example 3 does not control the content of the first component raw material in the raw material mixture, and does not control the oxygen content in the iron-platinum-based target; Comparative Examples 4 and 5 do not control the content of the nitride raw material in the raw material mixture, do not undergo the steps of water washing, drying, and hydrogen reduction, and do not control the oxygen content and calcium content in the iron-platinum-based target. The composition, calcium content and oxygen content of the FePt-based targets of Comparative Examples 2 to 5 are listed in Table 1-1, and the sintering process and sintering temperature are listed in Table 1-2.
比較例Comparison Example 66 至to 11 (C6-C11)11 (C6-C11) ：: 鐵鉑基靶材Iron platinum based target (( 含有碳Contains carbon ))
比較例6至11之鐵鉑基靶材所採用的方法與實施例15至20之鐵鉑基靶材的製備方法大致相同，其主要差異在於：比較例6、7未經過水洗、乾燥、和氫氣還原之步驟，以及未控制鐵鉑基靶材中的氧含量和鈣含量；比較例8未經過氫氣還原之步驟，以及未控制鐵鉑基靶材中的氧含量；比較例9未經過水洗、乾燥之步驟，以及未控制鐵鉑基靶材中的鈣含量；比較例10、11皆未控制原料混合物中第一成分原料含量、未經過水洗、乾燥、和氫氣還原之步驟，以及未控制鐵鉑基靶材中的氧含量和鈣含量。比較例6至11之鐵鉑基靶材的組成、鈣含量和氧含量皆列於表1-1中，而燒結製程以及燒結溫度則列於表1-2中。
表1-1 實施例1至20及比較例1至11之鐵鉑基靶材之組成、其鈣含量和氧含量
分析analyze 11 ：鐵鉑基靶材之鈣含量: Calcium content of FePt target
將實施例1至20與比較例1至11燒結後先得到的鐵鉑基合金粗胚，以線切割取得2公分(cm) × 2 cm的試片，再進行表面黑皮磨除及清洗處理。The iron-platinum-based alloy rough pieces obtained after sintering in Examples 1 to 20 and Comparative Examples 1 to 11 were cut by wire cutting to obtain 2 cm × 2 cm test pieces, and then the black skin on the surface was removed and cleaned.
隨後，將實施例1至20與比較例1至11之鐵鉑基靶材的試片置入輝光放電質譜儀(GD-MS)中並進行鈣含量的測定，並將測定結果記錄於表2中。Subsequently, the samples of the FePt-based targets of Examples 1 to 20 and Comparative Examples 1 to 11 were placed in a GD-MS to measure the calcium content, and the measurement results are recorded in Table 2.
分析analyze 22 ：鐵鉑基靶材之氧含量：Oxygen content of FePb-based target
將實施例1至20與比較例1至11燒結後先得到的鐵鉑基合金粗胚以線割加工，接著進行表面黑皮磨除及清洗處理後，各取50毫克(mg)至100 mg做為待測樣品。接著，將各組的待測樣品分別放置於石墨坩堝中，於持續通氦氣的氣氛下進行加熱燃燒，使前述待測樣品中的氧含量轉化為一氧化碳，最後利用氧氮分析儀(型號為HORIBA公司製造的EMGA-620W)以非分散紅外吸收法進行檢測，得到各待測樣品的氧含量，並將測定結果列於表2中。The iron-platinum-based alloy rough blanks obtained after sintering in Examples 1 to 20 and Comparative Examples 1 to 11 were processed by wire cutting, and then the black skin on the surface was removed and cleaned, and 50 mg to 100 mg of each were taken as the test samples. Then, the test samples of each group were placed in a graphite crucible, and heated and burned in a helium atmosphere to convert the oxygen content in the test samples into carbon monoxide. Finally, the oxygen and nitrogen analyzer (model EMGA-620W manufactured by HORIBA) was used to detect the oxygen content of each test sample by non-dispersive infrared absorption method, and the test results are listed in Table 2.
分析analyze 33 ：靶材相對密度: Target relative density
將實施例1至20與比較例1至11燒結後先得到的鐵鉑基合金粗胚，以線切割取得1cm × 1 cm的試片，再進行表面黑皮磨除及清洗處理，接著透過阿基米德法，得到實施例1至20與比較例1至11之鐵鉑基靶材的相對密度，並將結果記錄於表2中。The iron-platinum-based alloy rough blanks obtained after sintering of Examples 1 to 20 and Comparative Examples 1 to 11 were used to obtain 1 cm × 1 cm test pieces by wire cutting, and then the surface black skin was removed and cleaned. Then, the relative density of the iron-platinum-based target materials of Examples 1 to 20 and Comparative Examples 1 to 11 was obtained by the Archimedean method, and the results are recorded in Table 2.
分析analyze 44 ：靶材抗氧化能力：Target material antioxidant capacity
將實施例1至20與比較例1至11燒結後先得到的鐵鉑基合金粗胚以線切割取得5 cm × 5 cm的試片，再進行表面黑皮磨除及清洗處理。The iron-platinum-based alloy rough billets obtained after sintering in Examples 1 to 20 and Comparative Examples 1 to 11 were cut by wire cutting to obtain 5 cm × 5 cm test pieces, and then the black skin on the surface was removed and cleaned.
接著，將實施例1至20與比較例1至11之鐵鉑基靶材試片置於溫度為60℃、相對濕度為85%的高溫高濕環境中，並且每小時以放大倍率為100倍之光學顯微鏡(Optical Microscope，OM)檢驗各試片的表面是否出現氧化鏽斑的情況，直到試片表面出現目視明顯可見由於氧化所致的鏽蝕現象，記錄經過的總時間作為鏽斑出現時間。其中，以光學顯微鏡拍攝的影像圖如圖1、圖2所示，圖1是實施例1之鐵鉑基靶材試片經過172小時的抗氧化試驗後，以光學顯微鏡放大100倍的影像圖，而圖2是比較例4之鐵鉑基靶材試片經過2小時的抗氧化試驗後，以光學顯微鏡放大100倍的影像圖。明顯的，實施例1因氧化而出現鏽蝕現象的時間遠多於比較例4所需的時間。Next, the iron-platinum-based target specimens of Examples 1 to 20 and Comparative Examples 1 to 11 were placed in a high temperature and high humidity environment with a temperature of 60°C and a relative humidity of 85%, and the surface of each specimen was inspected every hour with an optical microscope (OM) with a magnification of 100 times to see if there was any rust spot, until the surface of the specimen showed obvious visual rust corrosion due to oxidation, and the total time elapsed was recorded as the rust spot appearance time. Among them, the images taken with an optical microscope are shown in Figures 1 and 2. Figure 1 is an image of the iron-platinum-based target material sample of Example 1 after 172 hours of anti-oxidation test, magnified 100 times by an optical microscope, and Figure 2 is an image of the iron-platinum-based target material sample of Comparative Example 4 after 2 hours of anti-oxidation test, magnified 100 times by an optical microscope. Obviously, the time for Example 1 to rust due to oxidation is much longer than the time required for Comparative Example 4.
「鏽斑出現時間」愈長，代表鐵鉑基靶材具有愈佳的抗氧化能力，「鏽斑出現時間」愈短，則表示鐵鉑基靶材的抗氧化能力愈差。實施例1至20與比較例1至11之鐵鉑基靶材在高溫高濕環境下之鏽斑出現時間列於表2中。在本創作中，鏽斑出現時間大於75小時被判定為通過抗氧化能力測試。The longer the "rust spot appearance time", the better the antioxidant ability of the iron platinum-based target material, and the shorter the "rust spot appearance time", the worse the antioxidant ability of the iron platinum-based target material. The rust spot appearance time of the iron platinum-based target materials of Examples 1 to 20 and Comparative Examples 1 to 11 in a high temperature and high humidity environment is listed in Table 2. In this work, a rust spot appearance time greater than 75 hours is judged to have passed the antioxidant ability test.
分析analyze 55 ：表面粗糙度:Surface roughness
將實施例1至20與比較例1至11之鐵鉑基靶材以線割與磨床加工後，製得直徑為3英吋、厚度為5 mm的圓形靶材，接著，將各靶材置於持續通有50 sccm (Standard Cubic Centimeter per Minute)之氬氣流量、0.001托耳(torr)至0.01 torr之真空度的磁控濺鍍機台(廠商：高敦)中，先以預濺鍍(pre-sputter)清除靶材表面的髒汙 (功率：100瓦(W)；時間：600秒)，獲得可進行後續濺鍍之待濺鍍靶材。接著，使該待濺鍍靶材置於通有50 sccm之氬氣流量、10 -2torr至10 -3torr之真空度的濺鍍環境下，以80 W之功率對直徑為2英吋、厚度為0.5 cm的玻璃試片進行600秒之濺鍍製程，進而各組分別獲得一濺鍍薄膜。 The iron platinum-based targets of Examples 1 to 20 and Comparative Examples 1 to 11 were processed by wire cutting and grinding to obtain circular targets with a diameter of 3 inches and a thickness of 5 mm. Then, each target was placed in a magnetron sputtering machine (manufacturer: Golden) with a continuous argon flow rate of 50 sccm (Standard Cubic Centimeter per Minute) and a vacuum degree of 0.001 torr to 0.01 torr. The dirt on the surface of the target was first removed by pre-sputtering (power: 100 watts (W); time: 600 seconds) to obtain a target to be sputtered for subsequent sputtering. Next, the target to be sputtered was placed in a sputtering environment with an argon gas flow rate of 50 sccm and a vacuum degree of 10 -2 torr to 10 -3 torr, and a sputtering process was performed for 600 seconds at a power of 80 W on a glass specimen with a diameter of 2 inches and a thickness of 0.5 cm, thereby obtaining a sputtered film for each group.
隨後，藉由形狀分析雷射共軛焦兼白光干涉顯微鏡 (型號：VK-X3000，製造商：KEYENCE)之三維(3D)影像功能，對各濺鍍薄膜表面根據ISO 25178標準方法進行表面粗糙度分析，以獲得各濺鍍薄膜之算術平均粗糙度(arithmetic mean deviation，Ra)以及最大高度(maximum height of profile，Rz)，各組之測量結果記錄於表2中。所述最大高度表示的是在基準長度上的粗糙度曲線中，最高波峰的高度與最深波谷的深度之和。Subsequently, the surface roughness of each sputtered film was analyzed according to the ISO 25178 standard method by using the three-dimensional (3D) imaging function of a shape analysis laser confocal white light interference microscope (model: VK-X3000, manufacturer: KEYENCE) to obtain the arithmetic mean deviation (Ra) and maximum height of profile (Rz) of each sputtered film. The measurement results of each group are recorded in Table 2. The maximum height represents the sum of the height of the highest peak and the depth of the deepest valley in the roughness curve on the reference length.
由於各濺鍍薄膜係以相同的濺鍍方法分別製得，故各濺鍍薄膜的表面粗糙度之差異主要係源自於濺鍍靶材之特性。在本創作中，單層的濺鍍薄膜之Ra小於20奈米(nm)且Rz小於50 nm被判定為通過表面粗糙度測試。
表2
實驗結果討論Experimental Results Discussion
根據各實施例的製備方法並配合表2的實驗結果可知，藉由至少同時採用(1)控制第一成分原料與氮化物原料的使用量範圍、(2)進行水洗、乾燥工序以及(3)經過氫氣還原再燒結等技術手段，使所製得之鐵鉑基靶材能同時兼具以下技術特徵：(I)所述第一成分含量大於或等於2 at%且小於或等於12 at%、(II)所述氮化物含量大於或等於8 at%且小於或等於30 at%、(III)鐵鉑基靶材中的鈣含量小於20 ppm、(IV)鐵鉑基靶材中的氧含量小於1000 ppm以及(Ⅴ)鐵鉑基靶材的相對密度大於98%。反觀各比較例並未同時採用前述技術手段(1)至(3)，因此比較例1至11之鐵鉑基靶材也未能同時兼具前述技術特徵(I)至(V)。據此，相較於比較例1至11，實施例1至20之鐵鉑基靶材在相同的高溫高濕環境下，實施例1至20之鐵鉑基靶材之鏽斑出現時間可延長至大於75小時；由此可見，本創作所提供之技術手段能有效提升抗氧化能力。According to the preparation methods of each embodiment and the experimental results in Table 2, it can be seen that by at least simultaneously adopting (1) controlling the usage range of the first component raw material and the nitride raw material, (2) performing water washing and drying steps, and (3) undergoing hydrogen gas reduction and re-sintering, the obtained iron-platinum-based target can simultaneously have the following technical characteristics: (I) the first component content is greater than or equal to 2 at% and less than or equal to 12 at%, (II) the nitride content is greater than or equal to 8 at% and less than or equal to 30 at%, (III) the calcium content in the iron-platinum-based target is less than 20 ppm, (IV) the oxygen content in the iron-platinum-based target is less than 1000 ppm, and (V) the relative density of the iron-platinum-based target is greater than 98%. On the other hand, the comparative examples do not simultaneously adopt the aforementioned technical means (1) to (3), so the iron platinum-based targets of comparative examples 1 to 11 also fail to simultaneously possess the aforementioned technical features (I) to (V). Therefore, compared with comparative examples 1 to 11, the iron platinum-based targets of embodiments 1 to 20 can extend the rust spot appearance time of the iron platinum-based targets of embodiments 1 to 20 to more than 75 hours under the same high temperature and high humidity environment; it can be seen that the technical means provided by the present invention can effectively enhance the antioxidant capacity.
此外，從表2的實驗結果可以看出，以實施例1至20之鐵鉑基靶材進行濺鍍所製得之濺鍍薄膜的Ra皆小於20 nm且Rz皆小於50 nm，顯示所得之濺鍍薄膜具有表面粗糙度小的表面。In addition, it can be seen from the experimental results in Table 2 that the Ra of the sputtered films obtained by sputtering the FePt-based targets of Examples 1 to 20 are all less than 20 nm and the Rz are all less than 50 nm, indicating that the obtained sputtered films have a surface with small surface roughness.
再進一步參看實施例1以及比較例1的組別，雖然實施例1與比較例1之鐵鉑基靶材具有相同主要組成成分，即皆表示為46Fe-25Pt-4Ru-1B-24AlN，然而，因比較例1未依序進行水洗、乾燥之工序，導致所製得的鐵鉑基靶材的鈣含量高達211.7 ppm，由此可證，經過水洗工序確實可降低原料混合物的鈣含量，使所述乾燥後的原料混合物的鈣含量可控制在小於20 ppm的範圍；此外，因比較例1未進行氫氣還原工序，導致所製得的鐵鉑基靶材的氧含量高達2001 ppm，由此可證，經過氫氣還原工序確實可降低還原材料的氧含量，使所製得的鐵鉑基靶材的氧含量可控制在小於1000 ppm的範圍。因此，實施例1之鐵鉑基靶材不論在相對密度(99.24%)、延緩氧化現象(172小時)的結果皆遠優於比較例1之鐵鉑基靶材(相對密度為87.65%；鏽斑出現時間為5小時)。再者，由實施例1之鐵鉑基靶材濺鍍形成的濺鍍薄膜所具有的表面粗糙度(Ra為6 nm；Rz為24 nm)亦皆明顯小於由比較例1之鐵鉑基靶材濺鍍形成的濺鍍薄膜(Ra為23 nm；Rz為87 nm)。由此可知，藉由控制鐵鉑基靶材的鈣含量、氧含量和相對密度於特定範圍之技術特徵，確實有助於提升鐵鉑基靶材的抗氧化能力，且由其濺鍍形成的濺鍍薄膜可具有更低的表面粗糙度。Further referring to the combination of Example 1 and Comparative Example 1, although the iron platinum-based targets of Example 1 and Comparative Example 1 have the same main components, i.e., both are expressed as 46Fe-25Pt-4Ru-1B-24AlN, however, since Comparative Example 1 does not perform the water washing and drying steps in sequence, the calcium content of the iron platinum-based target obtained is as high as 211.7 ppm. It can be proved that the water washing step can indeed reduce the calcium content of the raw material mixture, so that the calcium content of the raw material mixture after drying can be controlled within the range of less than 20 ppm; in addition, since Comparative Example 1 does not perform the hydrogen reduction step, the oxygen content of the iron platinum-based target obtained is as high as 2001 ppm, which proves that the oxygen content of the reduced material can be reduced through the hydrogen reduction process, so that the oxygen content of the prepared FePt target can be controlled within the range of less than 1000 ppm. Therefore, the FePt target of Example 1 is far superior to the FePt target of Comparative Example 1 (relative density is 87.65%; rust spot appearance time is 5 hours) in terms of relative density (99.24%) and delayed oxidation phenomenon (172 hours). Furthermore, the surface roughness of the sputtered film formed by sputtering the FePt-based target in Example 1 (Ra is 6 nm; Rz is 24 nm) is also significantly smaller than that of the sputtered film formed by sputtering the FePt-based target in Comparative Example 1 (Ra is 23 nm; Rz is 87 nm). It can be seen that by controlling the technical characteristics of the FePt-based target in a specific range, the oxidation resistance of the FePt-based target is indeed improved, and the sputtered film formed by sputtering can have a lower surface roughness.
另參看比較例6、比較例7的組別，雖比較例6和比較例7的鐵鉑基靶材皆具有符合本創作界定的第一成分和氮化物之含量範圍，但因為比較例6和比較例7的製備過程中並未依序進行水洗、乾燥、氫氣還原等工序，因此無法控制其鈣含量(小於20 ppm)和氧含量(小於1000 ppm)以及相對密度(小於98%)，致使比較例6和比較例7的鐵鉑基靶材的鏽斑出現時間明顯較短，表示其抗氧化力不夠好。再者，由比較例6和比較例7之鐵鉑基靶材濺鍍形成的濺鍍薄膜所具有的表面粗糙度較大，表示其表面的平整性不佳。Also refer to the groups of Comparative Examples 6 and 7. Although the iron-platinum-based targets of Comparative Examples 6 and 7 have the first component and nitride content ranges that meet the definition of the present invention, because the preparation processes of Comparative Examples 6 and 7 did not sequentially perform water washing, drying, hydrogen reduction and other steps, it is impossible to control their calcium content (less than 20 ppm) and oxygen content (less than 1000 ppm) and relative density (less than 98%), resulting in the rust spots of the iron-platinum-based targets of Comparative Examples 6 and 7 appearing for a significantly shorter time, indicating that their antioxidant capacity is not good enough. Furthermore, the sputtered films formed by sputtering the FePt-based targets in Comparative Examples 6 and 7 have a relatively large surface roughness, indicating that the surface flatness thereof is not good.
再進一步參看比較例8和比較例9的組別，比較例8之鐵鉑基靶材中的第一成分之含量、氮化物之含量以及鈣含量皆符合本創作所限定之範圍，然而，比較例8之鐵鉑基靶材因製備過程未經過氫氣還原工序，故其氧含量略高於本創作所限定之小於1000 ppm的特定範圍且所述鐵鉑基靶材具有的相對密度小於98%(97.83%)，導致比較例8之鐵鉑基靶材之鏽斑出現時間較短(70小時)，由此可知，比較例8之鐵鉑基靶材同樣無法具有較佳的抗氧化能力。此外，比較例9之鐵鉑基靶材中的第一成分之含量、氮化物之含量以及氧含量皆符合本創作所限定之範圍，然而，比較例9之鐵鉑基靶材因製備過程未經過水洗工序控制鈣含量，故其鈣含量略高於本創作所限定的小於20 ppm之特定範圍，且比較例9之鐵鉑基靶材未控制其相對密度，導致且其鏽斑出現時間為67小時，由此可知，比較例9之鐵鉑基靶材同樣無法具有較佳的抗氧化能力。Further referring to the groups of Comparative Examples 8 and 9, the content of the first component, the content of the nitride and the content of calcium in the iron-platinum-based target of Comparative Example 8 are all within the ranges defined by the present invention. However, since the preparation process of the iron-platinum-based target of Comparative Example 8 did not undergo a hydrogen reduction process, its oxygen content is slightly higher than the specific range of less than 1000 ppm defined by the present invention and the relative density of the iron-platinum-based target is less than 98% (97.83%), resulting in a shorter rust spot appearance time (70 hours) for the iron-platinum-based target of Comparative Example 8. Therefore, it can be seen that the iron-platinum-based target of Comparative Example 8 also cannot have better antioxidant ability. In addition, the content of the first component, the content of the nitride, and the content of oxygen in the iron-platinum-based target of Comparative Example 9 are all within the ranges specified by the present invention. However, since the iron-platinum-based target of Comparative Example 9 did not undergo a water washing process to control the calcium content during its preparation, its calcium content was slightly higher than the specific range of less than 20 ppm specified by the present invention. Furthermore, the iron-platinum-based target of Comparative Example 9 did not control its relative density, resulting in the appearance time of its rust spots being 67 hours. Therefore, it can be seen that the iron-platinum-based target of Comparative Example 9 also cannot have better antioxidant ability.
再進一步參看比較例2和比較例3的組別，比較例2之鐵鉑基靶材因第一成分之含量過低且氮化物之含量過高，因此，即便比較例2的製備過程有經過水洗、乾燥工序，仍無法將鐵鉑基靶材的鈣含量降低至小於20 ppm，導致由比較例2之鐵鉑基靶材濺鍍形成的濺鍍薄膜仍具有較大的表面粗糙度(Ra為20 nm；Rz為63 nm)。比較例3之鐵鉑基靶材因第一成分之含量過高，因此，即便比較例3的製備過程有經過氫氣還原工序，仍無法將鐵鉑基靶材的氧含量降低至小於1000 ppm，，導致比較例3之鐵鉑基靶材的抗氧化能力較低，且由比較例3之鐵鉑基靶材濺鍍形成的濺鍍薄膜仍具有較大的表面粗糙度(Rz為58 nm)。Further referring to the groups of Comparative Examples 2 and 3, the iron-platinum-based target of Comparative Example 2 has too low a content of the first component and too high a content of nitride. Therefore, even though the preparation process of Comparative Example 2 has undergone water washing and drying steps, it is still impossible to reduce the calcium content of the iron-platinum-based target to less than 20 ppm, resulting in the sputtered film formed by sputtering the iron-platinum-based target of Comparative Example 2 still having a relatively large surface roughness (Ra is 20 nm; Rz is 63 nm). Since the content of the first component in the iron-platinum-based target of Comparative Example 3 is too high, even if the preparation process of Comparative Example 3 has undergone a hydrogen reduction step, the oxygen content of the iron-platinum-based target cannot be reduced to less than 1000 ppm, resulting in a lower antioxidant capacity of the iron-platinum-based target of Comparative Example 3, and the sputtered film formed by sputtering the iron-platinum-based target of Comparative Example 3 still has a relatively large surface roughness (Rz is 58 nm).
此外，再觀表2的分析結果，實施例1至3、5、6、8至13、15至17、19、20之鐵鉑基靶材因其氧含量少於625 ppm，因此出現鏽斑的時間較長(109小時以上)；甚至，實施例1、3、5、6、8、12、13、15至17、20之鐵鉑基靶材因其氧含量少於510 ppm，因此出現鏽斑的時間更長(大於120小時)。In addition, looking at the analysis results in Table 2, the iron-platinum-based targets of Examples 1 to 3, 5, 6, 8 to 13, 15 to 17, 19, and 20 have a longer time for rust spots to appear (more than 109 hours) because their oxygen content is less than 625 ppm; even more, the iron-platinum-based targets of Examples 1, 3, 5, 6, 8, 12, 13, 15 to 17, and 20 have a longer time for rust spots to appear (more than 120 hours) because their oxygen content is less than 510 ppm.
綜上所述，本創作藉由適當控制鐵鉑基靶材之第一成分、氮化物、鈣與氧的含量以及相對密度，進而可達成提升鐵鉑基靶材的抗氧化能力，並且，由其濺鍍形成的濺鍍薄膜具有表面粗糙度低之優點。據此，本創作提供之鐵鉑基靶材不僅能提升濺鍍形成的磁記錄層之膜層品質與良率，還可避免保存不當極易氧化產生鏽蝕的問題，進一步提升其於商業上的價值。In summary, the invention can improve the anti-oxidation ability of the FePt-based target by properly controlling the content and relative density of the first component, nitride, calcium and oxygen of the FePt-based target, and the sputtered film formed by the sputtering has the advantage of low surface roughness. Therefore, the FePt-based target provided by the invention can not only improve the film quality and yield of the magnetic recording layer formed by sputtering, but also avoid the problem of rusting caused by oxidation due to improper storage, further improving its commercial value.
上述實施例僅係為了方便說明而舉例而已，惟該實施方式並非用以限定本創作之申請專利範圍；舉凡其他未悖離本創作揭示內容下所完成的變化、修飾等變更，均應包含於本創作涵蓋的專利範圍中。The above-mentioned embodiments are only given for the convenience of explanation, but the embodiments are not intended to limit the scope of the patent application of this creation; any other changes, modifications, etc. that do not deviate from the disclosed content of this creation should be included in the patent scope covered by this creation.
無。without.
圖1係實施例1之鐵鉑基靶材經過172小時的抗氧化試驗後，以光學顯微鏡放大100倍的影像圖。 圖2係比較例4之鐵鉑基靶材經過2小時的抗氧化試驗後，以光學顯微鏡放大100倍的影像圖 Figure 1 is an image of the iron-platinum-based target material of Example 1 after 172 hours of anti-oxidation test, magnified 100 times by an optical microscope. Figure 2 is an image of the iron-platinum-based target material of Comparative Example 4 after 2 hours of anti-oxidation test, magnified 100 times by an optical microscope
無。without.
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| CN1077603C (en) * | 1998-05-12 | 2002-01-09 | 住友金属矿山株式会社 | Recovering method of valuable composition from rare earth element-containing material and alloy powder obtained therefrom |
| TW201428739A (en) * | 2012-08-31 | 2014-07-16 | Jx Nippon Mining & Metals Corp | Fe-BASED MAGNETIC MATERIAL SINTERED BODY |
| US20150136592A1 (en) * | 2012-08-10 | 2015-05-21 | Mitsui Mining & Smelting Co., Ltd. | Sintered Body and Sputtering Target |
| CN111801184A (en) * | 2018-03-05 | 2020-10-20 | 全球先进金属美国股份有限公司 | Powder metallurgy sputtering target and method for producing the same |
| JP2021008641A (en) * | 2019-06-28 | 2021-01-28 | 田中貴金属工業株式会社 | Fe-Pt-BN-BASED SPUTTERING TARGET AND METHOD FOR MANUFACTURING THE SAME |
| TW202212581A (en) * | 2020-09-25 | 2022-04-01 | 光洋應用材料科技股份有限公司 | Fe-pt based sputtering target and method of preparing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1077603C (en) * | 1998-05-12 | 2002-01-09 | 住友金属矿山株式会社 | Recovering method of valuable composition from rare earth element-containing material and alloy powder obtained therefrom |
| US20150136592A1 (en) * | 2012-08-10 | 2015-05-21 | Mitsui Mining & Smelting Co., Ltd. | Sintered Body and Sputtering Target |
| TW201428739A (en) * | 2012-08-31 | 2014-07-16 | Jx Nippon Mining & Metals Corp | Fe-BASED MAGNETIC MATERIAL SINTERED BODY |
| CN111801184A (en) * | 2018-03-05 | 2020-10-20 | 全球先进金属美国股份有限公司 | Powder metallurgy sputtering target and method for producing the same |
| JP2021008641A (en) * | 2019-06-28 | 2021-01-28 | 田中貴金属工業株式会社 | Fe-Pt-BN-BASED SPUTTERING TARGET AND METHOD FOR MANUFACTURING THE SAME |
| TW202212581A (en) * | 2020-09-25 | 2022-04-01 | 光洋應用材料科技股份有限公司 | Fe-pt based sputtering target and method of preparing the same |
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