JP2008019164A - Superfine particulate cubic boron nitride sintered compact - Google Patents
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本発明は、ダイヤモンドに次ぐ硬度を持ち、鉄系金属に対してはダイヤモンドよりも安定であり、鉄系金属の切削工具、研削材等として従来の機械加工分野に技術革新をもたらすことが期待できる高純度超微粒子透光性立方晶窒化ホウ素（ｃＢＮ）焼結体とその製造方法に関する。 The present invention has hardness next to diamond, is more stable than diamond for iron-based metals, and can be expected to bring technological innovation to conventional machining fields as iron-based metal cutting tools, abrasives, etc. The present invention relates to a high-purity ultrafine particle translucent cubic boron nitride (cBN) sintered body and a method for producing the same.
鉄系金属の切削工具、研削材として多様な形態のｃＢＮ焼結体が用いられてきた。これらは鉄系材料の機械加工に優れた特徴を有し、現代の産業基盤である機械加工分野で重要な位置を占めている。これまでに用いられてきたｃＢＮ焼結体は４〜５万気圧領域において種々の焼結助剤と共に焼結した複合焼結体であり、ｃＢＮの含有量は約４０〜９０ｗｔ％程度まで種々のものが開発されている。切削工具として用いる際には被削材の特性に応じてｃＢＮの含有量が制御されているが、近年、ｃＢＮ含有量が１００％の高純度焼結体により優れた切削性能が現れることが見いだされている（非特許文献１）。 Various forms of cBN sintered bodies have been used as ferrous metal cutting tools and abrasives. These have excellent characteristics in machining of iron-based materials and occupy an important position in the machining field, which is the modern industrial base. The cBN sintered body that has been used so far is a composite sintered body that is sintered together with various sintering aids in the region of 40 to 50,000 atm. The content of cBN varies from about 40 to 90 wt%. Things are being developed. When used as a cutting tool, the content of cBN is controlled according to the characteristics of the work material, but in recent years, it has been found that excellent cutting performance appears with a high-purity sintered body having a cBN content of 100%. (Non-Patent Document 1).
ｃＢＮ含有量が１００％の高純度ｃＢＮ焼結体の合成方法として、六方晶などの低圧相窒化ホウ素を原料として、高圧高温度下で高圧相であるｃＢＮへの相転移を進めながら同時に焼結反応を進行させる反応焼結法と、予め調製したｃＢＮ結晶粒子を原料として焼結助剤無添加で焼結する直接焼結法が知られている。これらにより現在までに、７．７万気圧、２０００℃領域において構成粒子径が０．５μｍ程度までの緻密な透光性のｃＢＮ焼結体の合成が報告されている（非特許文献２，３）。 As a method for synthesizing a high-purity cBN sintered body having a cBN content of 100%, a low-pressure boron nitride such as hexagonal crystal is used as a raw material, and simultaneously sintering while proceeding a phase transition to a high-pressure phase cBN under high pressure and high temperature. There are known a reactive sintering method in which the reaction proceeds and a direct sintering method in which cBN crystal particles prepared in advance are used as a raw material and sintered without adding a sintering aid. Thus, synthesis of a dense translucent cBN sintered body having a constituent particle diameter of about 0.5 μm in the region of 77,000 atm and 2000 ° C. has been reported so far (Non-patent Documents 2 and 3). ).
一方、焼結体の強度は構成粒子径に依存することが知られているが、微粒子が緻密に焼結した組織では内在する微小亀裂のサイズが小さくなるために焼結体としての強度が向上することが知られている。また、焼結体を切削工具として使用する際には被削材の加工面の面粗さは焼結体の構成粒子径の大きさの影響を受ける。このため、材料の鏡面加工などの精密加工を目的とした場合、焼結体の粒子径は可能な限り微小であることが望まれる。 On the other hand, it is known that the strength of the sintered body depends on the constituent particle diameter. However, in the structure in which fine particles are densely sintered, the size of the microcrack is small, so the strength of the sintered body is improved. It is known to do. Further, when the sintered body is used as a cutting tool, the surface roughness of the work surface of the work material is affected by the size of the constituent particle diameter of the sintered body. For this reason, when aiming at precision processing, such as mirror finishing of materials, it is desirable that the particle diameter of the sintered body be as small as possible.
さらに、透光性のｃＢＮ焼結体の高強度化を図ることは、工業的な応用として切削工具のみならず、高強度の窓材等への応用など実用上の意義がある。しかしながら、現在までに得られている透光性の高純度ｃＢＮ焼結体の粒子径は微粒径のものでも０．５μｍ程度までであり、これより小さい粒子径の緻密な高純度焼結体の合成は報告されていない。 Furthermore, increasing the strength of a translucent cBN sintered body has practical significance such as application to not only cutting tools but also high-strength window materials as industrial applications. However, the particle size of the translucent high-purity cBN sintered body obtained so far is up to about 0.5 μm even if the particle size is fine, and the dense high-purity sintered body having a smaller particle diameter is smaller than this. The synthesis of has not been reported.
自動車産業に代表される機械加工工程の高効率化、環境保全を実現する上で、既存のｃＢＮ焼結体工具の特性向上が求められている。ｃＢＮ焼結体工具の特性向上には、焼結体構造の微細な制御が不可欠であり、そのためには微粒子が緻密に焼結したｃＢＮ含有量が１００％の高純度ｃＢＮ焼結体の供給が不可欠である。 In order to improve the efficiency of machining processes represented by the automobile industry and to preserve the environment, it is required to improve the characteristics of existing cBN sintered body tools. In order to improve the characteristics of the cBN sintered body tool, fine control of the structure of the sintered body is indispensable. For this purpose, the supply of a high-purity cBN sintered body having a cBN content of 100%, in which fine particles are densely sintered, is required. It is essential.
既存の技術による高純度ｃＢＮ焼結体の合成は７．７万気圧領域で進められているが、この際に合成可能な透光性高純度ｃＢＮ焼結体の構成粒子径は微粒径のものでも、０．５μｍ程度以上である。粒径０．１μｍ以下の微細な組織の高純度ｃＢＮ焼結体は得られておらず、精密切削用の高性能切削工具や高強度の窓材等への応用が進められていない。 The synthesis of the high-purity cBN sintered body by the existing technology is proceeding in the region of 77,000 atmospheres, but the constituent particle size of the translucent high-purity cBN sintered body that can be synthesized at this time is a fine particle size. Even a thing is about 0.5 micrometer or more. A high-purity cBN sintered body having a fine structure with a particle size of 0.1 μm or less has not been obtained, and its application to high-performance cutting tools for precision cutting, high-strength window materials, etc. has not been promoted.
すなわち、本発明が解決しようとする課題は、従来の高純度ｃＢＮ焼結体の合成技術ではなし得なかった、構成粒子径が０．１μｍ以下の微細な構造を有し、かつｃＢＮ含有量が１００％の高純度超微粒子ｃＢＮ焼結体に透光性を有さしめることにある。 That is, the problem to be solved by the present invention is a fine structure having a constituent particle diameter of 0.1 μm or less, which cannot be achieved by the conventional synthesis technique of high-purity cBN sintered bodies, and has a cBN content of The purpose is to make the 100% high-purity ultrafine particle cBN sintered body have translucency.
本発明のｃＢＮ含有量が１００％で、焼結体の平均粒子径が０．１μｍ以下の高純度超微粒子ｃＢＮ焼結体は、透光性を有していることを特徴とする。 The high-purity ultrafine particle cBN sintered body having a cBN content of 100% and an average particle diameter of the sintered body of 0.1 μm or less according to the present invention is translucent.
本発明では、密切削用の高性能切削工具や高強度の窓材等への応用が可能となった。 The present invention can be applied to high-performance cutting tools for dense cutting, high-strength window materials, and the like.
焼結体の構成粒子径は焼結温度の増加と共に粒成長により増大するため、ナノスケールオーダーの微細な粒子の焼結体を合成するためには焼結条件を低く抑えることが必要となる。７．７万気圧領域におけるこの合成温度下限は約２０００℃であり、この条件下で粒径０．５μｍ程度の高純度の透光性ｃＢＮ焼結体が合成されている。これより微細な粒径の焼結体を合成するためには粒成長を抑制する必要があり、このためには焼結温度を低減する必要がある。
物質の低圧相から高圧相への相転換挙動は圧力と温度に依存するが、窒化ホウ素の相転換挙動を６万気圧から９万気圧の領域にかけて吟味した。その結果、残留する低圧相が全て高圧相である立方晶相に転換する温度は圧力の上昇と共に減少することが見いだされた。すなわち、７．７万気圧よりも高い圧力のもとでは六方晶相から立方晶へ相転移完了温度が低減することになる。これにより合成温度を低減し、粒成長を抑制した超微粒子焼結体の合成が期待できる。そこで、圧力９．５万気圧領域で六方晶窒化ホウ素を原料としてｃＢＮ焼結体の合成実験を行った。
Since the constituent particle diameter of the sintered body increases with grain growth as the sintering temperature increases, it is necessary to keep the sintering conditions low in order to synthesize a sintered body of fine particles of nanoscale order. The lower limit of the synthesis temperature in the region of 77,000 atmospheres is about 2000 ° C., and a high-purity translucent cBN sintered body having a particle size of about 0.5 μm is synthesized under this condition. In order to synthesize a sintered body having a finer particle size than this, it is necessary to suppress grain growth, and for this purpose, it is necessary to reduce the sintering temperature.
The phase transformation behavior of the substance from the low pressure phase to the high pressure phase depends on the pressure and temperature, but the phase transformation behavior of boron nitride was examined in the region of 60,000 to 90,000 atmospheres. As a result, it has been found that the temperature at which the remaining low-pressure phase is converted into the cubic phase, which is the high-pressure phase, decreases with increasing pressure. That is, under the pressure higher than 77,000 atm, the phase transition completion temperature from the hexagonal phase to the cubic crystal is reduced. Thereby, synthesis | combination of the ultrafine particle sintered compact which reduced the synthesis temperature and suppressed grain growth can be expected. Then, the synthetic | combination experiment of the cBN sintered compact was performed by using hexagonal boron nitride as a raw material in the pressure range of 95,000 atm.
六方晶窒化ホウ素原料は焼結体又は六方晶窒化ホウ素粉末として市販されているものを使用できる。しかし、通常、原料である六方晶窒化ホウ素には主たる不純物として酸化ホウ素が含まれており、これは得られる焼結体の強度の低下の原因となる。このため、窒素気流中、２０００℃で２時間の熱処理を原料の六方晶窒化ホウ素に施し、原料中の酸素不純物濃度を当初の０．５％から一桁程度低減した。この脱酸素処理を施した六方晶窒化ホウ素を原料として、９．５万気圧、１０００℃から２０００℃の範囲で高圧処理し、得られた焼結体の特性を評価した。得られた焼結体は合成温度が１７００℃以上でｃＢＮ単相であり、透光性を呈していた。走査型電子顕微鏡（ＳＥＭ）及び透過型電子顕微鏡（ＩＥＭ）観察によると構成粒子径は０．１μｍ以下であり、均一な組織であった。Ｘ線回折ではｃＢＮ以外のいかなる相も観測されず、ビッカース硬度は試験荷重４９Ｎにおいて５５ＧＰａであり、通常の焼結助剤を用いたｃＢＮ焼結体を大きく上回る特性であった。 As the hexagonal boron nitride raw material, a commercially available sintered body or hexagonal boron nitride powder can be used. However, hexagonal boron nitride as a raw material usually contains boron oxide as a main impurity, which causes a decrease in strength of the obtained sintered body. For this reason, a heat treatment for 2 hours at 2000 ° C. was performed on the raw material hexagonal boron nitride in a nitrogen stream, and the oxygen impurity concentration in the raw material was reduced by an order of magnitude from the initial 0.5%. The hexagonal boron nitride subjected to the deoxygenation treatment was subjected to high pressure treatment in the range of 95,000 atm and 1000 ° C. to 2000 ° C., and the characteristics of the obtained sintered body were evaluated. The obtained sintered body had a synthesis temperature of 1700 ° C. or higher, was a cBN single phase, and exhibited translucency. According to observation with a scanning electron microscope (SEM) and a transmission electron microscope (IEM), the constituent particle diameter was 0.1 μm or less, and the structure was uniform. In X-ray diffraction, no phase other than cBN was observed, and the Vickers hardness was 55 GPa at a test load of 49 N, which was a characteristic greatly surpassing that of a cBN sintered body using a normal sintering aid.
なお、合成温度が１７００℃未満では低圧相ＢＮ成分が残留し、透過率の減少と共に硬度の減少が見られた。また、合成温度が１９００℃を超えると焼結体の透過率は増加するが、硬度の減少が見られた。組織観察によると粒子径１μｍ以上までの粒成長が観察された。 When the synthesis temperature was less than 1700 ° C., the low-pressure phase BN component remained, and a decrease in hardness was observed as the transmittance decreased. Further, when the synthesis temperature exceeded 1900 ° C., the transmittance of the sintered body increased, but a decrease in hardness was observed. According to the structure observation, grain growth up to a particle diameter of 1 μm or more was observed.
以上の実験から、六方晶窒化ホウ素を原料として、立方晶窒化ホウ素が熱力学的に安定な９．５万気圧、１７００℃以上１９００℃以下の圧力、温度条件で、立方晶相への高圧相転移を伴いながら助剤無添加で焼結することにより、平均粒子径０．１μｍ以下の緻密な組織を有する高純度高硬度透光性ｃＢＮ超微粒子焼結体が合成できることを見いだした。本発明は、この知見に基づいて成されたものである。なお、当該微粒焼結体を合成するための最適温度条件は、低圧相から高圧相への転換を完了させるための温度下限と粒成長を抑制するための温度上限の間となる。
この最適条件は圧力に依存しており、圧力が高いほど最適温度の幅を広く取ることができるため、９．５万気圧以上の圧力領域であれば当該微粒焼結体の合成が可能となる。通常、この種の高圧装置としては、ベルト型超高圧力発生装置が適するが、このような装置では１０万気圧程度までの高圧を発生することが可能である。他の方式の高圧発生装置（たとえば多面体型高圧装置など）を用いれば、より高い圧力発生は可能であるが、この場合の試料容積は１０ｍｍ３程度以下と小さくなる。このため工業生産としての経済性を考慮すれば、当該焼結体の合成条件の上限としては、ベルト型高圧装置を用いた１０万気圧程度でよい。
From the above experiment, using hexagonal boron nitride as a raw material, cubic boron nitride is thermodynamically stable at 95,000 atmospheres, at a pressure of 1700 ° C. to 1900 ° C., and a high pressure phase to the cubic phase. It has been found that a high-purity, high-hardness translucent cBN ultrafine particle sintered body having a dense structure with an average particle diameter of 0.1 μm or less can be synthesized by sintering without adding an auxiliary agent while being accompanied by a transition. The present invention has been made based on this finding. The optimum temperature condition for synthesizing the fine grain sintered body is between the lower temperature limit for completing the conversion from the low pressure phase to the high pressure phase and the upper temperature limit for suppressing grain growth.
This optimum condition depends on the pressure, and the higher the pressure, the wider the range of the optimum temperature. Therefore, the fine sintered body can be synthesized in the pressure range of 95,000 atm or more. . Normally, a belt-type ultrahigh pressure generator is suitable as this type of high-pressure device, but such a device can generate a high pressure up to about 100,000 atmospheres. If another type of high-pressure generator (for example, a polyhedral high-pressure device) is used, higher pressure can be generated, but the sample volume in this case is as small as about 10 mm 3 or less. For this reason, considering the economical efficiency as industrial production, the upper limit of the synthesis condition of the sintered body may be about 100,000 atm using a belt-type high-pressure apparatus.
すなわち、本発明は、低圧相窒化ホウ素を従来技術よりも高い圧力条件で処理することにより、従来技術、先行技術では得ることのできなかった、高純度超微粒子透光性焼結体を提供するものである。
以下、本発明を実施例及び図面に基づいて説明する。
That is, the present invention provides a high-purity ultrafine particle translucent sintered body that cannot be obtained by the prior art and the prior art by treating low-pressure phase boron nitride under a higher pressure condition than the prior art. Is.
Hereinafter, the present invention will be described based on examples and drawings.
真空中で１５００℃、窒素気流中で２０００℃の熱処理による脱酸素処理を施した六方晶窒化ホウ素焼結体（粒径約０．５μｍ）を高圧容器内のタンタルカプセルに充填し、ベルト型超高圧力発生装置により９．５万気圧、１７００℃、の圧力、温度条件で３０分間焼結した。この際に、いっさいのｃＢＮ焼結助剤は添加しなかった。昇温速度は５℃／分程度であった。５００℃／分程度で冷却後、除圧し試料を圧力容器内のタンタルカプセルと共に回収した。 A hexagonal boron nitride sintered body (particle size: about 0.5 μm) that has been deoxygenated by heat treatment at 1500 ° C. in a vacuum and 2000 ° C. in a nitrogen stream is filled into a tantalum capsule in a high-pressure vessel. Sintering was performed for 30 minutes under a pressure and temperature conditions of 95,000 atm and 1700 ° C. using a high pressure generator. At this time, no cBN sintering aid was added. The heating rate was about 5 ° C./min. After cooling at about 500 ° C./min, the pressure was released and the sample was collected together with the tantalum capsule in the pressure vessel.
機械的又は化学処理（弗酸−硝酸混液）によりタンタルカプセルを除去し試料を回収した。試料の評価はダイヤモンド砥粒による研磨を施した後に硬度測定、破面のＳＥＭ観察、ＴＥＭ観察、並びにＸ線回折による相の同定を行った。図１に示した焼結体のＸ線回折図形より、焼結体はｃＢＮ単相であり、図２及び図３のＳＥＭ及びＴＥＭ観察写真が示すように平均粒子径０．１μｍ以下の均一な組織を呈し、異常粒成長等による粗大な粒子は見られなかった。 The tantalum capsule was removed by mechanical or chemical treatment (hydrofluoric acid-nitric acid mixture), and the sample was collected. The samples were evaluated by hardness measurement, SEM observation of the fracture surface, TEM observation, and phase identification by X-ray diffraction after polishing with diamond abrasive grains. From the X-ray diffraction pattern of the sintered body shown in FIG. 1, the sintered body is a single phase of cBN, and as shown in the SEM and TEM observation photographs of FIGS. No coarse particles due to abnormal grain growth or the like were observed.
また、硬度試験により、ビッカース硬度５５ＧＰａ（荷重４９Ｎ）程度の高硬度高純度のｃＢＮ微粒子焼結体であることが示された。焼結体は図４に示すような光透過率の波長依存性を示した。焼結体の厚さが０．６ｍｍの場合、可視光領域（波長５００〜８００ｎｍ）から赤外領域（波長３０００ｎｍ）における光透過率が１０％程度であった。図４に併せて示した焼結体の光学顕微鏡写真に見られるような透光性を呈する。 In addition, the hardness test showed that it was a cBN fine particle sintered body having a high hardness and a high purity of about 50 GPa hardness (load 49 N). The sintered body showed the wavelength dependence of the light transmittance as shown in FIG. When the thickness of the sintered body was 0.6 mm, the light transmittance from the visible light region (wavelength 500 to 800 nm) to the infrared region (wavelength 3000 nm) was about 10%. It exhibits translucency as seen in the optical micrograph of the sintered body also shown in FIG.
比較例１
実施例１記載のプロセスにおいて焼結条件９．５万気圧、１６００℃以下では低圧相窒化ホウ素の成分が焼結体中に残留し、ｃＢＮ単相の焼結体とならなかった。また、焼結温度が１９００℃を超えると得られる焼結体はｃＢＮ単相で高純度であり、高い透光性を呈するが、組織には粒成長が観察され、焼結体の硬度も低下が見られた。
Comparative Example 1
In the process described in Example 1, under the sintering conditions of 95,000 atm and 1600 ° C. or lower, the low-pressure phase boron nitride component remained in the sintered body and did not become a cBN single-phase sintered body. In addition, when the sintering temperature exceeds 1900 ° C., the obtained sintered body is a single phase of cBN and is highly pure and exhibits high translucency, but grain growth is observed in the structure, and the hardness of the sintered body is also reduced. It was observed.
本発明の高純度微粒ｃＢＮ焼結体の製造法において、良好な焼結体組織を得るためには焼結温度が重要であることが比較例から明らかとなった。実施例並びに比較例は本発明において高純度超微粒透光性ｃＢＮ焼結体を作製する際に、従来技術よりも高い圧力条件で焼結温度を最適化することが重要であることを示している。 In the method for producing a high-purity fine grain cBN sintered body according to the present invention, it was revealed from a comparative example that the sintering temperature is important in order to obtain a good sintered body structure. The examples and comparative examples show that it is important to optimize the sintering temperature under higher pressure conditions than in the prior art when producing a high purity ultrafine translucent cBN sintered body in the present invention. Yes.
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