JP6048629B2 - 立方晶窒化硼素焼結体および被覆立方晶窒化硼素焼結体 - Google Patents
立方晶窒化硼素焼結体および被覆立方晶窒化硼素焼結体 Download PDFInfo
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- JP6048629B2 JP6048629B2 JP2016550650A JP2016550650A JP6048629B2 JP 6048629 B2 JP6048629 B2 JP 6048629B2 JP 2016550650 A JP2016550650 A JP 2016550650A JP 2016550650 A JP2016550650 A JP 2016550650A JP 6048629 B2 JP6048629 B2 JP 6048629B2
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- boron nitride
- cubic boron
- sintered body
- nitride sintered
- compound
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims description 169
- 229910052582 BN Inorganic materials 0.000 title claims description 168
- 150000001875 compounds Chemical class 0.000 claims description 107
- 239000002245 particle Substances 0.000 claims description 33
- 239000000203 mixture Substances 0.000 claims description 26
- 239000011248 coating agent Substances 0.000 claims description 23
- 238000000576 coating method Methods 0.000 claims description 23
- 239000011230 binding agent Substances 0.000 claims description 20
- 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 description 19
- 239000013078 crystal Substances 0.000 claims description 18
- 238000002441 X-ray diffraction Methods 0.000 claims description 16
- 230000005484 gravity Effects 0.000 claims description 13
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 12
- 239000010410 layer Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 229910052796 boron Inorganic materials 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 229910052735 hafnium Inorganic materials 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 229910052758 niobium Inorganic materials 0.000 claims description 4
- 239000002356 single layer Substances 0.000 claims description 4
- 229910052715 tantalum Inorganic materials 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 239000000843 powder Substances 0.000 description 38
- 238000005520 cutting process Methods 0.000 description 30
- 239000002131 composite material Substances 0.000 description 18
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 238000005259 measurement Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 238000012545 processing Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 229910010037 TiAlN Inorganic materials 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 230000017525 heat dissipation Effects 0.000 description 3
- 238000007733 ion plating Methods 0.000 description 3
- 150000004767 nitrides Chemical class 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 101700004678 SLIT3 Proteins 0.000 description 2
- 102100027340 Slit homolog 2 protein Human genes 0.000 description 2
- 101710133576 Slit homolog 2 protein Proteins 0.000 description 2
- 102100027339 Slit homolog 3 protein Human genes 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910008482 TiSiN Inorganic materials 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229940126214 compound 3 Drugs 0.000 description 1
- 229940125898 compound 5 Drugs 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910000816 inconels 718 Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- QRXWMOHMRWLFEY-UHFFFAOYSA-N isoniazide Chemical compound NNC(=O)C1=CC=NC=C1 QRXWMOHMRWLFEY-UHFFFAOYSA-N 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001883 metal evaporation Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
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Description
(1)立方晶窒化硼素を50体積%以上75体積%以下と、結合相および不可避不純物を25体積%以上50体積%以下とからなる立方晶窒化硼素焼結体であって、
前記結合相は、Al化合物とZr化合物とを含み、
前記Al化合物は、Al元素と、N、OおよびBからなる群から選択される少なくとも1種の元素とを含み、
前記Zr化合物は、Zr元素と、C、N、OおよびBからなる群から選択される少なくとも1種の元素とを含み、
前記立方晶窒化硼素焼結体の研磨面において、
前記Zr化合物の重心から前記Zr化合物と前記Zr化合物以外の組成の部分との境界に達し、放射状に等間隔に引かれた複数の線分の数をN(但し、Nは8以上とする)とし、
前記線分のうち、前記Zr化合物と前記Zr化合物以外の組成の部分との境界において、前記立方晶窒化硼素と接する前記線分の数をnとしたとき、
n/Nの関係が0.25以上0.8以下を満たすZr化合物の個数が、Zr化合物の総数に対して40%以上である立方晶窒化硼素焼結体。
(2)前記Zr化合物は、前記立方晶窒化硼素焼結体全体に対して1体積%以上4体積%以下である(1)の立方晶窒化硼素焼結体。
(3)前記立方晶窒化硼素の平均粒径が0.2μm以上0.8μm以下である(1)または(2)の立方晶窒化硼素焼結体。
(4)前記Zr化合物は、ZrB2とZrO2とを含み、
前記ZrO2の結晶構造が正方晶、または正方晶および立方晶の両方が混在した状態で形成されており、
X線回折における、前記ZrB2の(100)面のピーク強度をI1、前記正方晶ZrO2の(101)面のピーク強度をI2t、前記立方晶ZrO2の(111)面のピーク強度をI2cとしたとき、
I2tとI2cとの強度の合計に対するI1の強度の比[I1/(I2t+I2c)]が、
0.5以上5以下である(1)〜(3)のいずれかの立方晶窒化硼素焼結体。
(5)前記Al化合物は、Al2O3からなる(1)〜(4)のいずれかの立方晶窒化硼素焼結体。
(6)(1)〜(5)のいずれかの立方晶窒化硼素焼結体の表面に被膜を形成した被覆立方晶窒化硼素焼結体。
(7)前記被膜が、Ti、Zr、Hf、V、Nb、Ta、Cr、Mo、W、AlおよびSiからなる群から選択される少なくとも1種以上の元素と、C、N、OおよびBからなる群から選択される少なくとも1種以上の元素とからなる(6)の被覆立方晶窒化硼素焼結体。
(8)前記被膜が、単層膜または2層以上の積層膜である(6)または(7)の被覆立方晶窒化硼素焼結体。
(9)前記被膜全体の平均膜厚が0.5μm以上20μm以下である(6)〜(8)のいずれかの立方晶窒化硼素焼結体。
工程(A):平均粒径0.2〜0.8μmの立方晶窒化硼素30〜70体積%と、平均粒径0.4〜0.8μmの、Zr元素の炭化物、窒化物、炭窒化物、酸化物および硼化物から成る群より選択された少なくとも1種の粉末30〜70体積%とが配合(但し、これらの合計は100体積%である)される。
工程(B):工程(A)で配合された原料粉が、ZrO2製ボールを備えた湿式ボールミルにより5〜48時間混合される。
工程(C):工程(B)で得られた混合物が、所定の形状に成形されて仮焼結される。
工程(D):工程(C)で得られた成形体が、超高圧発生装置に入れられ、5.0〜6.5GPaの圧力、かつ1200〜1400度の範囲の焼結温度で30分間保持されて焼結される。
工程(E):工程(D)で得られた複合体が、超硬合金製乳鉢によって粉砕され、複合体粉末が作製される。
工程(F):工程(E)で得られた複合体粉末が、超硬合金製ボールを備えた湿式ボールミルにより、24〜96時間粉砕され、複合体粉末がさらに微粒にされる。
工程(G):工程(F)を経た複合体粉末が、比重分離され、その後、酸処理により超硬合金由来成分が除去される。
工程(H):工程(G)を経た複合体粉末2〜14体積%と、平均粒径0.2〜0.8μmの立方晶窒化硼素50〜75体積%と、平均粒径0.05〜3.0μmの、Al元素の窒化物、酸化物および硼化物から成る群より選択された少なくとも1種の粉末11〜46体積%と、平均粒径0.5〜5.0μmの、Al粉末3〜13体積%とが配合(但し、これらの合計は100体積%である)される。
工程(I):工程(H)で配合された原料粉が、Al2O3製ボールを備えた湿式ボールミルにより5〜24時間混合される。
工程(J):工程(I)で得られた混合物が、所定の形状に成形される。
工程(K):工程(J)で得られた成形体が、超高圧発生装置に入れられ、4.5〜6.0GPaの圧力、かつ1300〜1500度の範囲の焼結温度で所定の時間保持されて焼結される。
工程(A)では、立方晶窒化硼素粉末と、Zr元素の炭化物、窒化物、炭窒化物、酸化物および硼化物からなる群より選択された少なくとも1種の粉末が用いられる。これにより、立方晶窒化硼素とZr化合物とが互いに粒界で接触する複合体粉末が作製される。また、工程(A)では、立方晶窒化硼素の粒径を調整することができる。特に、CeO2、Y2O3、MgO、CaOなどの安定化剤が添加されたZrO2粉末が用いられると、靱性に優れる正方晶または立方晶が形成される。ZrO2粉末の一次粒子の平均粒径が30〜50nmであると、立方晶窒化硼素焼結体の組織中に、微細なZrO2が分散しやすくなるという効果がある。しかしながら、取り扱いのしやすさから、平均粒径30〜50nmのZrO2の一次粒子が凝集した平均粒径0.1〜2μmの二次粒子のZrO2粉末を用いることが好ましい。
外周連続切削(旋削)、
被削材:インコネル718、
被削材形状:円柱φ120mm×350mm、
切削速度:300m/min、
切込み:0.2mm、
送り:0.2mm/rev、
クーラント:湿式、
評価項目:試料が欠損または最大逃げ面摩耗幅が0.2mmに至ったときを工具寿命とし、工具寿命に達するまでの切削時間を測定した。
1 立方晶窒化硼素
2 Zr化合物
3 Al化合物
4 Zr化合物の重心
5 Zr化合物の重心からZr化合物以外の組成の部分までの線分
Claims (9)
- 立方晶窒化硼素を50体積%以上75体積%以下と、結合相および不可避不純物を25体積%以上50体積%以下とからなる立方晶窒化硼素焼結体であって、
前記結合相は、Al化合物とZr化合物とを含み、
前記Al化合物は、Al元素と、N、OおよびBからなる群から選択される少なくとも1種の元素とを含み、
前記Zr化合物は、Zr元素と、C、N、OおよびBからなる群から選択される少なくとも1種の元素とを含み、
前記立方晶窒化硼素焼結体の研磨面において、
前記Zr化合物の重心から前記Zr化合物と前記Zr化合物以外の組成の部分との境界に達し、放射状に等間隔に引かれた複数の線分の数をN(但し、Nは8以上とする)とし、
前記線分のうち、前記Zr化合物と前記Zr化合物以外の組成の部分との境界において、前記立方晶窒化硼素と接する前記線分の数をnとしたとき、
n/Nの関係が0.25以上0.8以下を満たすZr化合物の個数が、Zr化合物の総数に対して40%以上である立方晶窒化硼素焼結体。 - 前記Zr化合物は、前記立方晶窒化硼素焼結体全体に対して1体積%以上4体積%以下である請求項1に記載の立方晶窒化硼素焼結体。
- 前記立方晶窒化硼素の平均粒径が0.2μm以上0.8μm以下である請求項1または2に記載の立方晶窒化硼素焼結体。
- 前記Zr化合物は、ZrB2とZrO2とを含み、
前記ZrO2の結晶構造が正方晶、または正方晶および立方晶の両方が混在した状態で形成されており、
X線回折における、前記ZrB2の(100)面のピーク強度をI1、前記正方晶ZrO2の(101)面のピーク強度をI2t、前記立方晶ZrO2の(111)面のピーク強度をI2cとしたとき、
I2tとI2cとの強度の合計に対するI1の強度の比[I1/(I2t+I2c)]が、
0.5以上5以下である請求項1〜3のいずれか1項に記載の立方晶窒化硼素焼結体。 - 前記Al化合物は、Al2O3からなる請求項1〜4のいずれか1項に記載の立方晶窒化硼素焼結体。
- 請求項1〜5のいずれか1項に記載の立方晶窒化硼素焼結体の表面に被膜を形成した被覆立方晶窒化硼素焼結体。
- 前記被膜が、Ti、Zr、Hf、V、Nb、Ta、Cr、Mo、W、AlおよびSiからなる群から選択される少なくとも1種以上の元素と、C、N、OおよびBからなる群から選択される少なくとも1種以上の元素とからなる請求項6に記載の被覆立方晶窒化硼素焼結体。
- 前記被膜が、単層膜または2層以上の積層膜である請求項6または7に記載の被覆立方晶窒化硼素焼結体。
- 前記被膜全体の平均膜厚が0.5μm以上20μm以下である請求項6〜8のいずれか1項に記載の被覆立方晶窒化硼素焼結体。
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