JP5519875B1 - セラミックス焼結体及び接合体 - Google Patents
セラミックス焼結体及び接合体 Download PDFInfo
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- JP5519875B1 JP5519875B1 JP2013548691A JP2013548691A JP5519875B1 JP 5519875 B1 JP5519875 B1 JP 5519875B1 JP 2013548691 A JP2013548691 A JP 2013548691A JP 2013548691 A JP2013548691 A JP 2013548691A JP 5519875 B1 JP5519875 B1 JP 5519875B1
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- ceramic sintered
- sintered body
- zirconia
- tungsten carbide
- alumina
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- 239000000919 ceramic Substances 0.000 title claims abstract description 81
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 76
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 claims abstract description 40
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000013078 crystal Substances 0.000 claims abstract description 26
- 239000002245 particle Substances 0.000 claims abstract description 24
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 11
- 229910052726 zirconium Inorganic materials 0.000 claims description 11
- 238000005304 joining Methods 0.000 claims description 4
- 239000011195 cermet Substances 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 description 31
- 238000012360 testing method Methods 0.000 description 21
- 239000000463 material Substances 0.000 description 16
- 229910045601 alloy Inorganic materials 0.000 description 11
- 239000000956 alloy Substances 0.000 description 11
- 238000000034 method Methods 0.000 description 11
- 230000000694 effects Effects 0.000 description 10
- 230000003746 surface roughness Effects 0.000 description 10
- 239000010936 titanium Substances 0.000 description 10
- 238000011156 evaluation Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 238000012545 processing Methods 0.000 description 7
- 238000003754 machining Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000000498 cooling water Substances 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical class [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- 238000005219 brazing Methods 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 229910000816 inconels 718 Inorganic materials 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 238000013001 point bending Methods 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- 239000006104 solid solution Substances 0.000 description 3
- 238000005728 strengthening Methods 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 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 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 235000012255 calcium oxide Nutrition 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000007970 homogeneous dispersion Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910002077 partially stabilized zirconia Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 150000003754 zirconium Chemical class 0.000 description 1
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract
Description
本発明の一側面におけるセラミックス焼結体において、炭化タングステンの平均粒径が0.7μm以下であることが好ましい。この場合、耐欠損性及び耐摩耗性が一層向上する。
本発明のセラミックス焼結体はアルミナを含む。本発明のセラミックス焼結体において、例えば、炭化タングステン、ジルコニア以外の残部をアルミナとすることができる。アルミナを含むことにより、セラミックス焼結体が化学的に安定し、耐摩耗性が一層向上する。炭化タングステン、ジルコニア及びアルミナの平均粒径は、1μm以下であることが好ましい。この場合、セラミックス焼結体の硬度と強度が高くなり、また、耐欠損性が一層高くなる。なお、本発明における平均粒径は、鏡面研磨した焼結体をエッチング処理し、これをSEM観察した画像を基に行うインターセプト法で測定した値を意味する。
・セラミックス焼結体の高靭性化、低熱膨張化、及び高熱伝導化が実現される。
炭化タングステンの平均粒径は特に0.7μm以下であることが好ましい。炭化タングステンの平均粒径が小さいことにより、上記の分散効果が一層顕著になる。
本発明のセラミックス焼結体は、ジルコニアを5〜25vol%含有することにより、応力誘起変態を効果的に生じさせることが出来るため、破壊靭性が高い。また、通常は耐摩耗性や耐熱衝撃性に劣るジルコニアの含有量を25vol%以下にすることにより、耐摩耗性、及び耐熱衝撃性を切削加工などの使用上で問題ない程度にすることができる。なお、ジルコニアの含有量は、セラミックス焼結体の全体を100vol%としたときの量である。
本発明のセラミックス焼結体は、例えば、ウィスカー原料を用いないものとすることができる。この場合、セラミックス焼結体の製造コストが低くなる。
以下の3種類の原料粉末をそれぞれ所定量秤量し、アセトンとともに樹脂製のミルに投入し、アルミナ球石を用いて48時間粉砕を行って、スラリーを得た。
平均粒径0.1〜1.5μmの炭化タングステン粉末
平均粒径0.6μmのジルコニア粉末(安定化剤として0〜8mol%のイットリア含有)
得られたスラリーを湯煎してエタノールを抜気し、ふるい通しを行うことで混合粉末を得た。この混合粉末をカーボン型に充填し、ホットプレス焼成を行い、セラミックス焼結体を得た。ホットプレス焼成の条件は以下のとおりとした。
焼成時間:2時間
圧力:30MPa
雰囲気:Arガス
上記の製造方法において、原料粉末の配合比、炭化タングステン粉末の平均粒径、及びジルコニア粉末におけるイットリアの含有量を種々に変えて、表1に示す組成を満たすS1〜S20、S30〜S36のセラミックス焼結体を製造した。ただし、S35のみは、上述したホットプレス焼成の条件ではなく、急速昇温(30℃/min以上)により焼成した。
S1〜S20、S30〜S36のセラミックス焼結体における粒界をSTEMにて観察したところ、S35以外においては、アルミナと炭化タングステンとの粒界にジルコニウム元素が分布することを確認した。急速昇温により焼成したS35においては、アルミナと炭化タングステンとの粒界にジルコニウム元素は分布していなかった。
(1)3点曲げ強度、ビッカース硬度、破壊靱性の測定
S1〜S26、S30〜36のセラミックス焼結体のそれぞれについて、3×4×15mmの試験片を作製し、3点曲げ強度(スパン10mm)、ビッカース硬度、及び破壊靱性(IF法)を測定した。また、室温における熱伝導率、600℃における熱膨張率の測定を所定の形状で行った。また、市販のアルミナ/ウィスカー系工具(以下、S27とする)、サイアロン系工具(以下、S28とする)、アルミナ/TiC系工具(以下、S29とする)についても、同様に測定を行った。その結果を表2に示す。なお、表2において、3点曲げ強度は「曲げ強度」と表示し、ビッカース硬度は「硬度」と表示する。
S1〜S36のセラミックス焼結体のそれぞれについて、切削チップを作成し、切削試験を行った。切削試験は下記の2試験を行った。
(a)切削試験1(鋳鉄の断続加工試験)
(a−1)試験の条件
チップ#形状:SNGN432−TN
被削材:FC200
切削速度:200m/min
切込量:1.5mm
送り量:0.55〜0.75mm/rev.
冷却水:なし
(a−2)評価方法
送り量を固定して5パス加工して欠損しなかったら、0.05mm/rev.だけ送り量を高くして加工するということを、送り量が0.75mm/rev.になるまで繰り返し、欠損が生じた時点の送り量で耐欠損性を評価した。具体的には、表2の「切削試験1」の「送り量」の列において、各送り量で欠損が生じない場合を「○」と示し、欠損が生じた場合に「欠損」と示す。また、表2の「切削試験1」の「判定」の列に示すように、送り量が0.65mm/rev.までに欠損した場合は「×」、0.70mm/rev.で欠損した場合は「△」、0.75mm/rev.で欠損した場合は「○」、未欠損の場合は「◎」と評価した。
(a−3)試験結果
試験結果を上記表2に示す。S3〜6、10〜12、14、15、17、18、30〜32、34のセラミックス焼結体は、他に比べて、耐欠損性が高かった。
(b)切削試験2(耐熱合金の旋削加工試験)
(b−1)試験の条件
チップ形状:RCGX120700T01020
被削材:インコネル718鍛造品
切削速度:240〜480m/min
切込量:1.0mm
送り量:0.2mm/rev.
冷却水:あり
(b−2)評価方法
各速度で2パス加工した後の境界摩耗量、刃先状態(チッピングの有無など)、仕上げ面状態に基づき、仕上げ面の状態(きれいさ)を、○(良)、△(中間)、×(悪)の3段階で評価した。
(b−3)試験結果
試験結果を上記表2に示す。なお、表2において(F)はフレーキング発生を意味する。S3〜6、10〜12、14、15、17、18、30〜36のセラミックス焼結体は、他に比べて、耐欠損性及び耐摩耗性が高かった。また、S3〜6、10〜12、14、15、17、18、30〜36のセラミックス焼結体は、他に比べて、仕上げ面がきれいであった。
(1)S3〜6、10〜12、14、15、17、18、30〜36のセラミックス焼結体は、耐欠損性及び耐摩耗性において優れている。
(2)S3〜6、10〜12、14、15、17、18、30〜36のセラミックス焼結体はS27と比較して安価に製造できる。
(3)S3〜6、10〜12、14、15、17、18、30〜36のセラミックス焼結体を用いれば、耐熱合金の高速・高能率加工が可能となる。
(4)S3〜6、10〜12、14、15、17、18、30〜36のセラミックス焼結体を用いれば、仕上げ面精度を高くすることができる。
(5)S3〜6、10〜12、14、15、17、18、30〜36のセラミックス焼結体を用いれば、耐熱合金加工が可能となる。
まず、図1Aに示すように、前記実施例1のセラミックス焼結体S5から成る第1の部材1と、超硬合金(WCとコバルトバインダーから成るもの)から成る第2の部材3とをそれぞれ製造した。第1の部材1は三角柱形状を有している。第2の部材3の基本的な形状は直方体であり、その2つの頂点3A、3Bにおいて、第1の部材1の分だけ切り欠かれている。
(1)試験の条件
接合体5をチップとして用いて、以下の条件で仕上げ加工を行った。このとき、接合体5のうち、被削材に主として接触する部分は、第1の部材1とした。
切削速度:240m/min
切込量:0.4mm
送り量:0.15mm/rev.
冷却水:あり
(2)評価方法
仕上げ加工後、チップのVB摩耗量と、加工面の面粗度とを測定した。チップのVB摩耗量について、0.3mmを寿命の摩耗量とした。また、面粗度とは、加工面の凸部と凹部との距離であり、面粗度が小さいほど、加工面の状態は良好である。
(3)試験結果
接合体5のチップを用いた場合、3パスの加工後、VB摩耗量は寿命の摩耗量の1/2程度であり、5パスの加工後、VB摩耗量は寿命の摩耗量に達した。また、接合体5のチップを用いた場合、加工面の面粗度は顕著に小さかった。
(1)試験の条件
接合体5をチップとして用いて、以下の条件で仕上げ加工を行った。このとき、接合体5のうち、被削材に主として接触する部分は、第1の部材1とした。
被削材:インコネル718鍛造品
切削速度:360m/min
切込量:0.4mm
送り量:0.15mm/rev.
冷却水:あり
(2)評価方法
仕上げ加工後、チップのVB摩耗量と、加工面の面粗度とを測定した。チップのVB摩耗量について、0.3mmを寿命の摩耗量とした。また、面粗度とは、加工面の凸部と凹部との距離であり、面粗度が小さいほど優れている。
(3)試験結果
接合体5のチップを用いた場合、2パスの加工後、VB摩耗量は寿命の摩耗量の1/2以下であり、4パスの加工後であっても、VB摩耗量は寿命の摩耗量に達しなかった。また、接合体5のチップを用いた場合、加工面の面粗度は顕著に小さかった。
接合体5は、高負荷及び高温状態においても、耐欠損性及び耐摩耗性において優れている。よって、接合体5を用いれば、耐熱合金に対する高能率の切削加工が可能になる。また、接合体5を用いれば、加工面の状態を改善することができる。
例えば、接合体5の形状は上述したものには限定されず、図2Aに示す形状(下方にゆくほど縮径した円柱形状)の第1の部材1及び第2の部材3をロウ付けにより接合し、図2Bに示す形状の接合体5を製造してもよい。また、第2の部材3の材質はサーメットであってもよい。
また、本発明のセラミックス焼結体は、例えば、摩擦攪拌接合や耐衝撃部材として用いることができる。
Claims (4)
- 炭化タングステン、ジルコニア、及びアルミナを含み、
炭化タングステンの含有量が20〜50vol%であり、
ジルコニアの含有量が5〜25vol%であり、
ジルコニアの結晶相が正方晶、又は正方晶と単斜晶との混晶であり、
Tiの化合物を実質的に含まず、
炭化タングステンの平均粒径、ジルコニアの平均粒径及びアルミナの平均粒径がともに1μm以下であることを特徴とするセラミックス焼結体。 - 炭化タングステンの平均粒径が0.7μm以下であることを特徴とする請求項1に記載のセラミックス焼結体。
- アルミナと炭化タングステンとの粒界にジルコニウム元素が分布することを特徴とする請求項1又は2に記載のセラミックス焼結体。
- 請求項1〜3のいずれか1項に記載のセラミックス焼結体から成る第1の部材と、超硬合金又はサーメットから成る第2の部材とを接合した接合体。
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JP2001019537A (ja) * | 1999-06-30 | 2001-01-23 | Ngk Spark Plug Co Ltd | エッジ付きセラミック部材 |
JP2002194474A (ja) * | 2000-12-22 | 2002-07-10 | Ngk Spark Plug Co Ltd | 炭化タングステン系超硬基複合材料焼結体 |
JP2010235351A (ja) * | 2009-03-30 | 2010-10-21 | Ngk Spark Plug Co Ltd | アルミナ基セラミック焼結体、切削インサート及び切削工具 |
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US11111182B2 (en) | 2015-12-07 | 2021-09-07 | Tungaloy Corporation | Ceramic sintered body |
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JPWO2014002743A1 (ja) | 2016-05-30 |
EP2772472B1 (en) | 2017-07-26 |
US20140242383A1 (en) | 2014-08-28 |
EP2772472A4 (en) | 2015-04-22 |
CN103974922A (zh) | 2014-08-06 |
EP2772472A1 (en) | 2014-09-03 |
US8927447B2 (en) | 2015-01-06 |
CA2877623A1 (en) | 2014-01-03 |
ES2643898T3 (es) | 2017-11-27 |
WO2014002743A1 (ja) | 2014-01-03 |
CA2877623C (en) | 2015-11-24 |
KR101522147B1 (ko) | 2015-05-20 |
CN103974922B (zh) | 2015-08-05 |
KR20140069090A (ko) | 2014-06-09 |
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