JP2020515490A - 焼結多結晶立方晶窒化ホウ素材料 - Google Patents
焼結多結晶立方晶窒化ホウ素材料 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 31
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 13
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 239000011159 matrix material Substances 0.000 claims abstract description 59
- 239000002245 particle Substances 0.000 claims abstract description 46
- 238000000034 method Methods 0.000 claims abstract description 35
- 239000000843 powder Substances 0.000 claims abstract description 26
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 11
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- -1 aluminum compound Chemical class 0.000 claims abstract description 3
- 238000003801 milling Methods 0.000 claims description 12
- 239000010936 titanium Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000009826 distribution Methods 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 claims description 2
- 229910033181 TiB2 Inorganic materials 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 150000003609 titanium compounds Chemical class 0.000 claims 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 claims description 2
- 238000005245 sintering Methods 0.000 description 28
- 238000007906 compression Methods 0.000 description 13
- 239000000203 mixture Substances 0.000 description 13
- 239000000523 sample Substances 0.000 description 12
- 238000003754 machining Methods 0.000 description 11
- 230000008569 process Effects 0.000 description 11
- 230000015572 biosynthetic process Effects 0.000 description 10
- 230000006835 compression Effects 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 9
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- 238000005520 cutting process Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000005553 drilling Methods 0.000 description 4
- 230000002829 reductive effect Effects 0.000 description 4
- 238000004626 scanning electron microscopy Methods 0.000 description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 229910003460 diamond Inorganic materials 0.000 description 3
- 239000010432 diamond Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
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- 239000013074 reference sample Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 229910000760 Hardened steel Inorganic materials 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
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- 230000009036 growth inhibition Effects 0.000 description 2
- 230000000670 limiting effect Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
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- 238000009700 powder processing Methods 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000012935 Averaging Methods 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 206010010144 Completed suicide Diseases 0.000 description 1
- 229910001263 D-2 tool steel Inorganic materials 0.000 description 1
- BRDWIEOJOWJCLU-LTGWCKQJSA-N GS-441524 Chemical compound C=1C=C2C(N)=NC=NN2C=1[C@]1(C#N)O[C@H](CO)[C@@H](O)[C@H]1O BRDWIEOJOWJCLU-LTGWCKQJSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
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- 229910052796 boron Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000011195 cermet Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
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- 150000001247 metal acetylides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1436—Composite particles, e.g. coated particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23B—TURNING; BORING
- B23B27/00—Tools for turning or boring machines; Tools of a similar kind in general; Accessories therefor
- B23B27/14—Cutting tools of which the bits or tips or cutting inserts are of special material
- B23B27/148—Composition of the cutting inserts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
- B28B11/24—Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
- B28B11/243—Setting, e.g. drying, dehydrating or firing ceramic articles
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- C04B35/645—Pressure sintering
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
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- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B10/00—Drill bits
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
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- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
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Abstract
Description
研磨材成形体は、切削、ミリング、研削、ドリル加工、および他の研磨作業に広く用いられている。それらは、一般的に、第二相マトリックス中に分散された超高硬度研磨材粒子を含有する。マトリックスは、金属、またはセラミック、またはサーメットであり得る。超高硬度研磨材粒子は、ダイヤモンド、立方晶窒化ホウ素(cBN)、炭化ケイ素、または窒化ケイ素などであり得る。これらの粒子は、一般的に用いられる高圧および高温の成形体製造プロセスの過程で互いに結合して、多結晶塊を形成してよく、または第二相材料のマトリックスを介して結合して、焼結多結晶体を形成してもよい。そのような多結晶体は、一般的に、PCDまたはPCBNとして知られ、これらはそれぞれ、超高硬度研磨材としてダイヤモンドまたはcBNを含有する。
米国特許第4,334,928号は、20〜80体積%の立方晶窒化ホウ素から本質的になり、残量は、周期律表のIVa族またはVa族遷移金属の炭化物、窒化物、炭窒化物、ホウ化物、およびケイ化物、これらの混合物、ならびにこれらの固溶体化合物からなる群より選択される少なくとも1つのマトリックス化合物材料のマトリックスである、工具に用いるための焼結成形体を教示している。マトリックスは、焼結体中の連続結合構造を形成し、高圧窒化ホウ素が、連続マトリックス内に点在している。この特許で概説される方法はすべて、ボールミリング、乳鉢などの機械的ミリング/混合法を用いて所望される材料を組み合わせることを含んでいる。
マトリックス相のための前駆体粉末は、より密接に混合する目的で、および粒子が小さい方が反応性が高いことから、粒子間の結合を改善する目的で、ミリングによってその粒子サイズが減少される。しかし、PCBNのための典型的な焼結プロセスでは、PCBN材料を形成するために、少なくとも1100℃の温度および少なくとも3.5GPaの圧力が用いられる。これらの条件下では、結晶粒の成長が発生する可能性があり、マトリックス粒子の一部の粒子サイズが大きく増加して、典型的には、1μmまでのサイズを有するようになる可能性がある。これは、得られるPCBNの特性に対して有害な影響を有する。
圧力は、少なくとも1GPaであってもよい。
温度は、1400℃以下および1300℃以下のいずれかから選択されてもよい。
時間は、2分間以下であってもよい。
方法は、さらに、毎分100〜500℃の加熱速度でその温度まで昇温することを含んでもよい。
マトリックス材料は、炭窒化チタン、炭化チタン、窒化チタン、二ホウ化チタン、窒化アルミニウム、および酸化アルミニウムのいずれかを含んでもよい。
マトリックス粉末およびcBN粉末を混合する工程は、湿式音響混合、乾式音響混合、およびアトリションミリングのいずれかを含んでもよい。
方法は、1μm超および4μm超のいずれかから選択される平均サイズを有するcBN粒子を提供することを含んでもよい。
方法は、多峰性平均サイズ分布を有するcBN粒子を提供することを含んでもよい。
以降では、添付の図面を参照して、限定されない実施形態を、例として記載する。
切片長さ法を用いる場合、顕微鏡写真にランダムな直線を描き、その線と交差する結晶粒界の数をカウントする。平均結晶粒サイズは、交差数を実際の線の長さで除することによって見出される。2本以上のランダムな線を用いて結果を平均することで、結果の精度が向上する。平均結晶粒サイズは、以下の数式によって与えられる。
同様に、ある特定の条件下における放電プラズマ焼結(SPS)も、結晶粒の成長を制限することが見出された。結晶粒の成長を制限することは、マトリックス相中の結晶粒が小さくなると、PCBNから製造される工具の特性が向上することから、有利である。そのような特性としては、工具の増加およびクレータ摩耗の低減が挙げられる。
マトリックス相がTiC0.5N0.5Alであり1.3μmのcBN含有量が55体積%である粉末組成物を、アトリションミリングによる粉末処理経路を介して調製した。粉末を約8トンで金属カップにプレスして、17mm径のグリーン体を製造し、ベルト型高圧高温装置中で焼結した。
粉末の焼結は、表1に示されるように、5つの異なる焼結サイクルを用いて行った。各焼結サイクルにおいて、19分間の最高温度での保持時間を用いた。
多くの切削作業では、工具は、連続および断続モードでパーツを機械加工することが要求される。工作物形状におけるギャップまたは空間は、断続として知られ、断続の連続機械加工に対する長さの比が、切削関与角と共に、機械加工作業における断続の度合いを決定する。
中断続適用(H15/H20)では、化学摩耗は、深いクレータ形成をもたらす結果となり、これは、PCBN工具が機械加工中の工作物のギャップまたは中断に遭遇した場合に欠けのリスクのあるシャープエッジを作り出す。このことは、中断続適用において大きな課題を課すものであり、PCBN工具の成功は、耐化学摩耗性と耐衝撃性または衝撃強度とのバランスに依存する。
中断続機械加工試験(断続スケール上でのH15領域)を、ドリルであけた孔が6つあるAISI4340硬化鋼工作物を用い、150m/分の表面切削速度で、0.15mm/回転の送り速度および0.2mmの切削深さによって行った。PCBN工具のエッジは、20μm研磨砥石を用いてSNMN090308 S0220試料エッジ仕様に調製した。
低断続機械加工試験(断続スケール上でのH10領域)を、H15試験に類似の条件を用いたが、6つ孔の面の代わりに3つ孔の面を用いて行った。
図2は、3つ孔のドリル加工試験においてH10条件を用いて試験した場合の、例1および3のクレータ摩耗を比較したものである。これは、例3よりも高い圧力で焼結した例1において、クレータ摩耗が著しく低減されたことを示している。
シェラーの計算法を用いて、例1〜5についてXRDピークの幅とマトリックス相中の結晶子のサイズとを関連付けた。表2に示した結果から、温度が、セラミックマトリックスの結晶子サイズに影響を与える最も著しい因子であることが示された。しかし、最も小さい結晶子サイズは、最も高い圧力で焼結した場合に得られたことも分かる。圧力よりも温度の方が、結晶子サイズに対して影響が大きいことが分かる。焼結された結晶粒は、2つ以上の結晶子からなり得ることから、結晶子サイズは、結晶粒サイズよりも小さい場合があることには留意されたい。
表3に示されるように、3つの異なる焼結サイクル、および2つの異なるcBN含有量を用いて、これらの粉末を焼結した。各例において、試料は、最高温度で19分間保持した。
これらの試料を、SEMを用いて分析して、セラミックマトリックス相の粒子サイズ分布を推定した。表4は、選択された例のマトリックス相の平均粒子サイズを示す。
高cBN含有量および低cBN含有量である粉末組成の2つの変型例を選択した。高含有量変型例(例9)では、平均粒子サイズ10μmのcBNが90質量%、および平均粒子サイズ6μmのアルミニウムが10質量%であった。81gの10μm cBNおよび9gのアルミニウムを、共振音響ミキサーを80Gで2分間用いて混合した。
予備圧縮のための3つの経路、セラミックカップへのハンド圧縮、キュービックプレスでの冷間圧縮、続いて最後に、再度キュービックプレスでの熱間圧縮、を選択し、3工程のプロセスとなった。しかし、cBN含有量がより低い変型例(例10)では、冷間圧縮の前に液圧圧縮を試行したため、例10(ハンド圧縮)と例11(液圧圧縮)とを区別した。圧縮工程を、図5にまとめる。
セラミックカップを、外側エンベロープに配置し、この段階での焼結を避けるために直接の加熱を行うことなく、キュービックプレスを用いてプレスした。試料は、600MPaでプレスした。試料を取り出し、次に1300℃、1800℃、および2000℃で、約7GPaの圧力下、熱間圧縮を行った。
熱間圧縮後に密度を測定すると、例9は、3.36g/cm3の最終密度を有し、例10および11は、3.67g/cm3の最終密度を有していた。より高い密度は、セラミックTiC0.5N0.5マトリックスおよびそのより高い密度の結果である。
それらのhBNカップから、研削によってスラグを取り出した。次に、得られたシリンダーを、研削によって平滑仕上げした。これに続いて、回転スピンドルおよびレーザーを用いて、それらをスライスしてディスクとした。ディスクを3.2mmの高さまで重ね、摩耗試験用に10×10mmの正方形を切り出した。SEM分析用に研磨するために、追加のピースを切り出した。
例10および11の場合、スラグは、カップから取り出す際に壊れた。これらのピースは、摩耗試験用に回収することはできなかったが、小ピースを、SEMによって分析した。
焼結温度は、cBNがマトリックス相と反応する速度を変化させる。例10および11の場合、図6に示されるように、焼結温度が上昇すると、ホウ素がマトリックス相へ拡散する速度の上昇に恐らくは起因して、ホウ化物相が広がることが分かる。このことは、50.7°2θのcBNピークの存在の減少によっても示される。また、より高い温度では、AlNの相対強度の減少も見られ、Alのホウ化物形成に有利である可能性がある。
図7は、1300℃および2000℃で焼結した例9のXRDスペクトルを示す。ここでは、AlNの形成が大きく増加している以外、相違点はほとんど見られない。ホウ化物相は検出されなかった。
図8は、高断続条件下、送り速度0.3mm、深さ0.2mm、切削速度180m/分、およびD2工具鋼の工作物材料を用いて試験した場合の、1300℃、1800℃、および2000℃で焼結した例9の工具寿命を示す。2000℃で焼結した材料から製造された試料は、僅かに1パス後に工具破壊を起こした。この非常に脆弱な挙動は、マトリックス相中での反応の広がり、および結晶粒の過剰な成長に起因し得る。
放電プラズマ焼結(SPS)は、PCBNの迅速な焼結を可能とする技術である。パルスDC電流がグリーン体に適用され、非常に高い加熱および冷却速度が可能となる。プロセスが迅速であることにより、焼結プロセスの過程での結晶粒の成長を最小限に抑えながら、迅速な高密度化が可能となる。PCBNに適用された場合のSPSのさらなる利点は、その迅速性によって、そうでなければ比較的低圧力(3GPa未満)で発生することになるcBNのhBNへの変換が低減されることである。
初期実験を行い、約30体積%超のcBN含有量および5〜10μmよりも微細であるSPS焼結試料が、著しいhBN形成という結果であったことが示された。
表5は、80MPaの圧力でSPSを用いて調製したPCBNに対する例示的データを示し、表6は、様々な圧力でSPSを用いて調製したPCBNに対する例示的データを示す。試料はすべて、85質量%TiC/15質量%Alのマトリックス中のcBNの体積%を示し、80MPa試料に対しては20mmの試料サイズで、他の試料に対しては6mmの試料サイズで行った。
さらに、表5に示される密度データから、SPSプロセスの過程における高密度化の度合い、およびさらには、nBNの形成の度合いの両方が示され、その理由は、hBNが約2.1gcm-3の密度を有し、cBNが約3.45gcm-3の密度を有することから、密度が低い方が、hBN変換の度合いが高いことを示しているからである。
表5および6ならびに図11および12に報告したPCBN成形体の結果から考えて、cBN含有量は、引き続き30体積%以下に維持し、平均粒子サイズ10μmを用いた。焼結の時間および圧力は、表7に示されるように変化させた。
図11は、例35〜43に対するビッカース硬度データを示し、図12は、例44〜53に対するビッカース硬度データを示す。図11から、より高い圧力が、恐らくは高密度化の向上の結果として、硬度を向上させていることが分かり、一方図12では、より高い圧力が、硬度を低下させたことが分かる。これは、バインダー化学の違いによって引き起こされたものと考えられ、この原因では、残留ケイ素化合物の形成が、材料をより脆弱とする可能性がある。
平均粒子サイズ10μmのcBN粒子を含むcBN含有量が30体積%の粉末を、アトリションミリング経路によって調製した。マトリックス材料の組成は、85質量%のTi(C0.5N0.5)0.8および15質量%の70mol% Al/30mol% Tiの組み合わせとした。マトリックス材料を、まず、真空中、1050℃で熱処理し、続いて、ヘキサン中でのアトリションミリングを4時間行った。cBNをアトリションミリング混合物に添加し、さらに10分間混合した。
最終混合物を乾燥し、80MPaおよび1GPaの2つの異なる圧力レベルが可能であるSPSプレス中、グラファイトカッピングの構成で焼結した。用いた加熱速度は、100℃/分であり、冷却速度は、200℃/分であった。表8に示されるように、SPSの異なる時間および最高温度を用いた。
最終混合物を乾燥し、80MPaおよび1GPaの2つの異なる圧力レベルが可能であるSPSプレス中、グラファイトカッピングの構成で焼結した。用いた加熱速度は、100℃/分であり、冷却速度は、200℃/分であった。表9に示されるように、SPSの異なる時間および最高温度を用いた。
図18は、例62の走査型電子顕微鏡写真であり、結晶粒の均一な分布を示している。以下の表10は、選択された例のマトリックス結晶粒サイズを示す。
Al(金属形態、または予備反応された形態のいずれか)が、安全上の理由から、マトリックス前駆体粉末中において粗くてもよく(>100nm)、このことが、前駆体粉末のd90値を高めることに繋がることには留意されたい。しかし、焼結の過程において、Alは溶融し、続いて固化してより小さい粒子サイズとなる。この理由から、出発粉末は、マトリックスの得られた結晶粒サイズよりも高いd90値を有し得る。
本明細書で用いられる場合、PCBN材料とは、金属またはセラミックを含むマトリックス中に分散されたcBNの結晶粒を有する超高硬度材料の一種を意味する。
本明細書で用いられる場合、「PCBN構造」は、PCBN材料体を含む。
「マトリックス材料」は、多結晶構造中の細孔、間隙、もしくは間隙領域を完全にまたは部分的に埋めるマトリックス材料を意味するものと理解される。「マトリックス前駆体粉末」の用語は、高圧高温焼結プロセスに掛けられた場合にマトリックス材料となる粉末を意味するために用いられる。
本発明について、実施形態を参照して特に示し、記載してきたが、当業者であれば、添付の特許請求の範囲によって規定される本発明の範囲から逸脱することなく、形式上および詳細な様々な変更を行ってよいことは理解される。例えば、例はすべて、cBNを超高硬度相として用いているが、マトリックス材料中に分散された他の種類の超高硬度材料に対しても、同じ方法が用いられ得ることは理解される。
Claims (11)
- 多結晶立方晶窒化ホウ素(PCBN)材料を製造する方法であって、
250nm以下の平均粒子サイズを有する粒子を含み、アルミニウム化合物を含むマトリックス前駆体粉末を、30〜40体積パーセントの、少なくとも4μmの平均粒子サイズを有する立方晶窒化ホウ素(cBN)粒子と混合する工程と、
前記混合された粒子を、少なくとも500MPaの圧力、1050℃以上〜1500℃以下の温度および1分間以上〜3分間以下の時間で放電プラズマ焼結する工程と
を含む、方法。 - 前記圧力が、少なくとも1GPaである、請求項1に記載の方法。
- 前記温度が、1400℃以下および1300℃以下のいずれかから選択される、請求項1または2に記載の方法。
- 前記時間が、2分間以下である、請求項1から3までのいずれか1項に記載の方法。
- 毎分100〜500℃の加熱速度で前記温度まで昇温することをさらに含む、請求項1から4までのいずれか1項に記載の方法。
- マトリックス材料が、さらに、炭素および窒素のいずれかのチタン化合物を含む、請求項1から5までのいずれか1項に記載の方法。
- マトリックス材料が、炭窒化チタン、炭化チタン、窒化チタン、二ホウ化チタン、窒化アルミニウム、および酸化アルミニウムのいずれかを含む、請求項1から6までのいずれか1項に記載の方法。
- マトリックス粉末およびcBN粉末を密接に混合する工程が、湿式音響混合、乾式音響混合、およびアトリションミリングのいずれかを含む、請求項1から7までのいずれか1項に記載の方法。
- 0.2〜15μmの平均サイズを有するcBN粒子を提供することを含む、請求項1から8までのいずれか1項に記載の方法。
- 1μm超および4μm超のいずれかから選択される平均サイズを有するcBN粒子を提供することを含む、請求項1から9までのいずれか1項に記載の方法。
- 多峰性平均サイズ分布を有するcBN粒子を提供することを含む、請求項1から10までのいずれか1項に記載のPCBN材料を製造する方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GBGB1704133.6A GB201704133D0 (en) | 2017-03-15 | 2017-03-15 | Sintered polycrystalline cubic boron nitride material |
GB1704133.6 | 2017-03-15 | ||
PCT/EP2018/056168 WO2018167017A1 (en) | 2017-03-15 | 2018-03-13 | Sintered polycrystalline cubic boron nitride material |
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DE102019207350A1 (de) * | 2019-05-20 | 2020-11-26 | Siemens Aktiengesellschaft | Schweißverfahren mit ummantelten abrasiven Teilchen, ummanteltes abrasives Teilchen, Schichtsystem und Dichtungssystem |
JP6912685B2 (ja) * | 2019-07-18 | 2021-08-04 | 住友電気工業株式会社 | 立方晶窒化硼素焼結体 |
JP6908798B2 (ja) * | 2019-07-18 | 2021-07-28 | 住友電気工業株式会社 | 立方晶窒化硼素焼結体 |
CN114144391B (zh) * | 2019-07-18 | 2023-04-18 | 住友电气工业株式会社 | 立方晶氮化硼烧结体 |
KR102244550B1 (ko) * | 2019-12-24 | 2021-04-26 | 고등기술연구원연구조합 | 합금 분말을 이용한 비정질 연자성 코어 제조 방법 및 비정질 연자성 코어 |
US11866372B2 (en) | 2020-05-28 | 2024-01-09 | Saudi Arabian Oil Company | Bn) drilling tools made of wurtzite boron nitride (W-BN) |
CN111805701A (zh) * | 2020-08-05 | 2020-10-23 | 江苏新伊菲科技有限公司 | 一种智能热压成型军用防护陶瓷的设备 |
CN112658261B (zh) * | 2020-12-09 | 2023-04-07 | 北京阿尔玛斯科技有限公司 | 聚晶立方氮化硼刀具及其制备方法 |
US11572752B2 (en) | 2021-02-24 | 2023-02-07 | Saudi Arabian Oil Company | Downhole cable deployment |
US11727555B2 (en) | 2021-02-25 | 2023-08-15 | Saudi Arabian Oil Company | Rig power system efficiency optimization through image processing |
US11846151B2 (en) | 2021-03-09 | 2023-12-19 | Saudi Arabian Oil Company | Repairing a cased wellbore |
US11624265B1 (en) | 2021-11-12 | 2023-04-11 | Saudi Arabian Oil Company | Cutting pipes in wellbores using downhole autonomous jet cutting tools |
US11867012B2 (en) | 2021-12-06 | 2024-01-09 | Saudi Arabian Oil Company | Gauge cutter and sampler apparatus |
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DE19845151A1 (de) * | 1998-10-01 | 2000-04-06 | Martin Kraemer | Verfahren zur Herstellung von verschleißfesten Verbundwerkstoffen |
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GB2560641A (en) | 2018-09-19 |
US20200071583A1 (en) | 2020-03-05 |
GB201704133D0 (en) | 2017-04-26 |
CN110494579A (zh) | 2019-11-22 |
GB2560642B (en) | 2020-06-17 |
KR20220143772A (ko) | 2022-10-25 |
CN110431247A (zh) | 2019-11-08 |
KR20190127809A (ko) | 2019-11-13 |
GB201803981D0 (en) | 2018-04-25 |
EP3596244A1 (en) | 2020-01-22 |
GB2560641B (en) | 2019-12-25 |
EP3596243A1 (en) | 2020-01-22 |
JP7053653B2 (ja) | 2022-04-12 |
GB201803960D0 (en) | 2018-04-25 |
GB2560642A (en) | 2018-09-19 |
US20210403385A1 (en) | 2021-12-30 |
JP2020514235A (ja) | 2020-05-21 |
WO2018167022A1 (en) | 2018-09-20 |
WO2018167017A1 (en) | 2018-09-20 |
KR20190126861A (ko) | 2019-11-12 |
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