JP2020203821A - Cr−Si系焼結体 - Google Patents
Cr−Si系焼結体 Download PDFInfo
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- JP2020203821A JP2020203821A JP2019203770A JP2019203770A JP2020203821A JP 2020203821 A JP2020203821 A JP 2020203821A JP 2019203770 A JP2019203770 A JP 2019203770A JP 2019203770 A JP2019203770 A JP 2019203770A JP 2020203821 A JP2020203821 A JP 2020203821A
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- Prior art keywords
- sintered body
- less
- based sintered
- powder
- silicon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229910019819 Cr—Si Inorganic materials 0.000 title claims abstract description 34
- 239000011651 chromium Substances 0.000 claims abstract description 37
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 31
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 19
- 239000010703 silicon Substances 0.000 claims abstract description 19
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000013078 crystal Substances 0.000 claims abstract description 9
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 7
- CHXGWONBPAADHP-UHFFFAOYSA-N [Si].[Si].[Cr] Chemical compound [Si].[Si].[Cr] CHXGWONBPAADHP-UHFFFAOYSA-N 0.000 claims abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 16
- 239000001301 oxygen Substances 0.000 claims description 16
- 229910052760 oxygen Inorganic materials 0.000 claims description 16
- 238000005477 sputtering target Methods 0.000 claims description 15
- 229910019974 CrSi Inorganic materials 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 238000004544 sputter deposition Methods 0.000 claims description 6
- 239000010409 thin film Substances 0.000 claims description 6
- 238000005452 bending Methods 0.000 claims description 4
- 229910021357 chromium silicide Inorganic materials 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 39
- 239000000843 powder Substances 0.000 description 29
- 238000002844 melting Methods 0.000 description 21
- 230000008018 melting Effects 0.000 description 21
- 238000010304 firing Methods 0.000 description 20
- 239000002245 particle Substances 0.000 description 19
- 239000012535 impurity Substances 0.000 description 14
- 238000009689 gas atomisation Methods 0.000 description 11
- 239000002994 raw material Substances 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 10
- 239000002184 metal Substances 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000010949 copper Substances 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 5
- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229910021332 silicide Inorganic materials 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 230000006837 decompression Effects 0.000 description 4
- 229910052748 manganese Inorganic materials 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000007751 thermal spraying Methods 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 238000007088 Archimedes method Methods 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000002742 anti-folding effect Effects 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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Abstract
Description
(1)Cr(クロム)、シリコン(Si)を含むCr−Si系焼結体であり、X線回折で帰属される結晶構造がクロムシリサイド(CrSi2)、シリコン(Si)から構成され、CrSi2相がバルク中に60wt%以上存在し、焼結体密度が95%以上であり、CrSi2相の平均粒径が60μm以下であることを特徴とするCr−Si系焼結体。
(2)抗折強度が100MPa以上であることを特徴とする(1)に記載のCr−Si系焼結体。
(3)バルク中の酸素量が1wt%以下であることを特徴とする(1)又は(2)に記載のCr−Si系焼結体。
(4)(1)〜(3)のいずれかに記載のCr−Si系焼結体からなることを特徴とするスパッタリングターゲット。
(5)(4)に記載のスパッタリングターゲットを用いてスパッタリングすることを特徴とする薄膜の製造方法。
原料はクロム、シリコンを用いる。原料の純度は99.9%以上が好ましく、より好ましくは99.99%以上である。不純物が多く含まれると、焼成工程における異常粒成長の原因や成膜の時のパーティクルの発生源となる。また、原料の酸素量は少ない物が好ましい。原料中の酸素量が多いと最終的にスパッタリングターゲット中の酸素量が多くなり、パーティクルの発生の原因となる。
次に得られた粉末をホットプレス炉等加圧焼成炉を使用すること好ましい。無加圧炉では、シリコンの拡散係数が低いことから高密度化するのが困難である。
(1)焼結体の密度
焼結体の相対密度は、JIS R 1634に準拠して、アルキメデス法によりかさ密度を測定し、真密度で割って相対密度を求めた。焼結体の真密度は、CrSi2相の重量a[g]およびSi相の重量をb[g]と、それぞれの真密度4.98[g/cm3]、2.3[g/cm3]を用いて、下記式で表される相加平均より算出した。
d=(a+b)/((a/4.98)+(b/2.3)
(2)X線回折試験
鏡面研磨した焼結体試料の2θ=20〜70°の範囲のX線回折パターンを測定した。
X線源 :CuKα
パワー :40kV、40mA
ステップ幅:0.01°
(3)焼結体粒径
鏡面研磨し、走査電子顕微鏡で観察し、得られた焼結体組織画像から直径法で焼結体粒径を測定した。少なくとも任意の3点以上を観察し、300個以上の粒子の測定を行った。
(走査電子顕微鏡の観察条件)
加速電圧 :10kV
(4)抗折強度
JIS R 1601に準拠して測定した。
(抗折強度の測定条件)
試験方法 :3点曲げ試験
支点間距離 :30mm
試料サイズ :3×4×40mm
ヘッド速度 :0.5mm/分。
(5)酸素量の分析
焼成後の焼結体表面より1mm以上研削した後の任意の部分より切り出したサンプルの分析値を測定データとした。
装置 :LECO TC436 酸素・窒素分析装置
(6)金属不純物量の分析
焼成後の焼結体表面より1mm以上研削した後の任意の部分より切り出したサンプルの分析値を測定データとした。
(実施例1)
Crフレーク(4N):42wt%、Siフレーク(5N):58wt%をカーボンルツボ内で溶解し、溶融温度を1650℃としてガスアトマイズ法により粉末を作製した。粉末を大気下で篩(篩目サイズ:300μm)により粉末の粒度調整を実施した。
(焼成条件)
焼成炉 :ホットプレス炉
昇温速度 :200℃/時間
昇温雰囲気:真空減圧雰囲気
焼成温度 :1250℃
圧力 :10MPa
焼成時間 :3時間
焼結体サイズ53mmΦ×7mmtのマイクロクラックのない焼結体が得られた。焼結体特性を表1に示す。
焼成条件を変更した以外は、実施例1と同様の方法で焼結体を作製した。焼結体の焼結体特性を表1に示す。
Crフレーク(4N):29wt%、Siフレーク(5N):71wt%を出力100Aの条件でアーク溶解法により溶解した。得られたバルクを乳鉢で粉砕し、実施例3の条件で焼成した。焼結体の特性を表1に示す。
Crフレーク(4N):42wt%、Siフレーク(5N):58wt%をカーボンルツボ内で溶解し、溶融温度を1650℃としてガスアトマイズ法により粉末を作製した粉末をグローブボックス内(酸素濃度:0.1wt%以下)で篩(篩目サイズ:300μm)により粉末の粒度調整を実施した。
(焼成条件)
焼成炉 :ホットプレス炉
昇温速度 :200℃/時間
昇温雰囲気:真空減圧雰囲気
焼成温度 :1200℃
圧力 :20MPa
焼成時間 :3時間
焼結体サイズ53mmΦ×7mmtのマイクロクラックのない焼結体が得られた。焼結体特性を表1に示す。
(実施例8)
Crフレーク(4N):29wt%、Siフレーク(5N):71wt%をカーボンルツボ内で溶解し、溶融温度を1540℃としてガスアトマイズ法により粉末を作製した粉末をグローブボックス内(酸素濃度:0.1wt%以下)で篩(篩目サイズ:300μm)により粉末の粒度調整を実施した。
(焼成条件)
焼成炉 :ホットプレス炉
昇温速度 :200℃/時間
昇温雰囲気:真空減圧雰囲気
焼成温度 :1200℃
圧力 :20MPa
焼成時間 :3時間
焼結体サイズ53mmΦ×7mmtのマイクロクラックのない焼結体が得られた。焼結体特性を表1に示す。 また、金属不純物量をGDMS分析し、Cr、Si以外の金属不純物総量は0.026wt%以下であり、個々の不純物量はFeが0.0027wt%、Niが0.00039wt%、Alが0.000022wt%、Mnが0.000041wt%、Cuが0.000012wt%であった。
(実施例9)
焼成条件を変更した以外は、実施例8と同様の方法で焼結体を作製した。焼結体の焼結体特性を表1に示す。
(実施例10)
Crフレーク(4N):47wt%、Siフレーク(5N):53wt%をカーボンルツボ内で溶解し、溶融温度を1540℃としてガスアトマイズ法により粉末を作製した粉末をグローブボックス内(酸素濃度:0.1wt%以下)で篩(篩目サイズ:300μm)により粉末の粒度調整を実施した。
(焼成条件)
焼成炉 :ホットプレス炉
昇温速度 :200℃/時間
昇温雰囲気:真空減圧雰囲気
焼成温度 :1200℃
圧力 :20MPa
焼成時間 :3時間
焼結体サイズ53mmΦ×7mmtのマイクロクラックのない焼結体が得られた。焼結体特性を表1に示す。 また、金属不純物量をGDMS分析し、Cr、Si以外の金属不純物総量は0.03wt%以下であり、個々の不純物量はFeが0.0062wt%、Niが0.00078wt%、Alが0.000035wt%、Mnが0.000068wt%、Cuが0.000041wt%であった。
焼成条件を変更した以外は、実施例10と同様の方法で焼結体を作製した。焼結体の焼結体特性を表1に示す。
(比較例1)
Crフレーク(4N):42wt%、Siフレーク(5N):58wt%をアーク溶解法で溶解した。溶解後得られたバルクの特性を表1に示す。
(比較例2)
比較例1で作製したバルクを乳鉢で粉砕し、ホットプレス法により作製した。焼結体特性を表1に示す。
(比較例3)
Cr粉末(45μm)、Si粉末(9μm)をV型混合法により混合し、混合粉をホットプレスし、焼結体を作製した。焼結体特性を表1に示す。
(比較例4)
ガスアトマイズ法により作製した粉末を焼成条件を変更して焼成を行った。焼結体特性を表1に示す。
(比較例5)
Crフレーク(4N):29wt%、Siフレーク(5N):71wt%をアーク溶解法で溶解した。溶解後得られたバルクの特性を表1に示す。
Claims (5)
- Cr(クロム)、シリコン(Si)を含むCr−Si系焼結体であり、X線回折で帰属される結晶構造がクロムシリサイド(CrSi2)、シリコン(Si)から構成され、CrSi2相がバルク中に60wt%以上存在し、焼結体密度が95%以上であり、CrSi2相の平均粒径が60μm以下であることを特徴とするCr−Si系焼結体。
- 抗折強度が100MPa以上であることを特徴とする請求項1に記載のCr−Si系焼結体。
- バルク中の酸素量が1wt%以下であることを特徴とする請求項1又は2に記載のCr−Si系焼結体。
- 請求項1〜3のいずれかに記載のCr−Si系焼結体からなることを特徴とするスパッタリングターゲット。
- 請求項4に記載のスパッタリングターゲットを用いてスパッタリングすることを特徴とする薄膜の製造方法。
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WO2022210428A1 (ja) * | 2021-03-29 | 2022-10-06 | 東ソー株式会社 | Cr-Si系膜 |
JP2022159957A (ja) * | 2021-04-05 | 2022-10-18 | Jx金属株式会社 | スパッタリングターゲット及びその製造方法 |
JP7494567B2 (ja) | 2020-05-26 | 2024-06-04 | 東ソー株式会社 | Cr-Si系焼結体 |
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JPWO2021241522A1 (ja) * | 2020-05-26 | 2021-12-02 | ||
KR20230043785A (ko) * | 2020-07-31 | 2023-03-31 | 도소 가부시키가이샤 | Cr-Si-C 계 소결체 |
CN112376023A (zh) * | 2020-11-04 | 2021-02-19 | 宁波江丰电子材料股份有限公司 | 一种铬硅合金溅射靶材的制备方法 |
CN113897585B (zh) * | 2021-10-11 | 2022-06-17 | 芜湖映日科技股份有限公司 | 一种硅铬旋转溅射靶材及其制备方法 |
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JPS5837274B2 (ja) * | 1980-08-26 | 1983-08-15 | 工業技術院長 | 高強度複合焼結材料 |
JP2570404B2 (ja) * | 1988-10-21 | 1997-01-08 | 三菱マテリアル株式会社 | NaおよびK含有量の少ないクロムシリサイド粉末の製造法 |
JPH03105901A (ja) * | 1989-09-20 | 1991-05-02 | Hitachi Ltd | 薄膜抵抗体とその製造法 |
JPH05214523A (ja) * | 1992-02-05 | 1993-08-24 | Toshiba Corp | スパッタリングターゲットおよびその製造方法 |
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JP4135357B2 (ja) * | 2001-11-30 | 2008-08-20 | 日鉱金属株式会社 | 金属シリサイドスパッタリングターゲット及びその製造方法 |
JP2004204278A (ja) | 2002-12-25 | 2004-07-22 | Hitachi Metals Ltd | シリサイドターゲット材の製造方法 |
KR100952889B1 (ko) * | 2005-06-15 | 2010-04-16 | 닛코킨조쿠 가부시키가이샤 | 스퍼터링 타겟트용 산화크롬 분말 및 스퍼터링 타겟트 |
BR112012003224A2 (pt) | 2009-08-21 | 2016-03-01 | Massachusetts Inst Technology | ligas ricas em silício |
CN105331939B (zh) * | 2014-08-15 | 2018-05-11 | 安泰科技股份有限公司 | 一种含硅合金靶材及其制备方法 |
JP6677883B2 (ja) | 2015-10-30 | 2020-04-08 | 三菱マテリアル株式会社 | スパッタリングターゲット及びスパッタリングターゲットの製造方法 |
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JP7494567B2 (ja) | 2020-05-26 | 2024-06-04 | 東ソー株式会社 | Cr-Si系焼結体 |
WO2022210428A1 (ja) * | 2021-03-29 | 2022-10-06 | 東ソー株式会社 | Cr-Si系膜 |
JP2022159957A (ja) * | 2021-04-05 | 2022-10-18 | Jx金属株式会社 | スパッタリングターゲット及びその製造方法 |
JP7394085B2 (ja) | 2021-04-05 | 2023-12-07 | Jx金属株式会社 | スパッタリングターゲット及びその製造方法 |
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