WO2020174921A1 - Nitrure de bore cubique polycristallin et procédé de production associé - Google Patents

Nitrure de bore cubique polycristallin et procédé de production associé Download PDF

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Publication number
WO2020174921A1
WO2020174921A1 PCT/JP2020/001436 JP2020001436W WO2020174921A1 WO 2020174921 A1 WO2020174921 A1 WO 2020174921A1 JP 2020001436 W JP2020001436 W JP 2020001436W WO 2020174921 A1 WO2020174921 A1 WO 2020174921A1
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Prior art keywords
boron nitride
cubic boron
temperature
pressure
polycrystal
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PCT/JP2020/001436
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English (en)
Japanese (ja)
Inventor
倫子 松川
久木野　暁
泰助 東
真知子 阿部
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住友電工ハードメタル株式会社
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Priority to CN202080010567.0A priority Critical patent/CN113329985A/zh
Priority to US17/052,920 priority patent/US11208324B2/en
Priority to EP20762962.7A priority patent/EP3932893A4/fr
Priority to PCT/JP2020/008149 priority patent/WO2020175642A1/fr
Priority to JP2020541821A priority patent/JP6798090B1/ja
Priority to KR1020217026969A priority patent/KR102685440B1/ko
Publication of WO2020174921A1 publication Critical patent/WO2020174921A1/fr

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    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
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    • B23B—TURNING; BORING
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Definitions

  • the present disclosure relates to a cubic boron nitride polycrystal and a method for manufacturing the same.
  • This application claims the priority right based on Japanese Patent Application No. 2 0 1 9 -0 3 6 2 6 1 filed on February 28, 2019 in Japan. All contents described in the Japanese patent application are incorporated herein by reference.
  • Cubic boron nitride (hereinafter, also referred to as " ⁇ mi 1 ⁇ 1”) has hardness second only to diamond, and is also excellent in thermal stability and chemical stability. Therefore, cubic boron nitride sintered bodies have been used as a material for tools.
  • the cubic boron nitride sintered body one containing a binder of about 10 to 40% by volume has been used.
  • the binder has been a cause of lowering the strength and thermal diffusivity of the sintered body.
  • a hexagonal boron nitride was directly converted into cubic boron nitride at ultrahigh pressure and high temperature without using a binder, and at the same time, the hexagonal boron nitride was sintered at the same time, so that the binder-free cubic
  • a method for obtaining a crystalline boron nitride sintered body has been developed.
  • Patent Document 1 discloses that a low crystalline hexagonal boron nitride is directly converted into a cubic boron nitride sintered body under ultrahigh temperature and high pressure, Moreover, a technique for obtaining a cubic boron nitride sintered body by sintering is disclosed.
  • Patent Document 1 Japanese Patent Laid-Open No. 1 1 -2 4 6 2 7 1
  • a cubic boron nitride polycrystalline body of the present disclosure is
  • a cubic boron nitride polycrystal containing 98.5% by volume or more of cubic boron nitride ⁇ 2020/174921 2 ⁇ (:171? 2020/001436
  • the dislocation density of the cubic boron nitride is greater than 8 ⁇ 10 15 / 2 , the cubic boron nitride polycrystal includes a plurality of crystal grains,
  • the cubic boron nitride polycrystalline body has a circle-equivalent median diameter 50 of the plurality of crystal grains of not less than 0.1 and not more than 0.5.
  • the hexagonal boron nitride powder is heated to a temperature of 1 700° ⁇ or more and 2500° ⁇ or less and a pressure of 80 3 or more by passing through the temperature and pressure in the stable region of wurtzite type boron nitride.
  • the stable region of the wurtzite boron nitride is
  • the plunge temperature of the wurtzite type boron nitride into the stable region is 500° or less
  • the heating and pressurizing step is a method for producing a cubic boron nitride polycrystal, which includes the step of maintaining the temperature and pressure in the stable region of the wurtzite boron nitride for 10 minutes or more.
  • Fig. 1 is a pressure-temperature phase diagram of boron nitride.
  • FIG. 2 is a diagram for explaining an example of a method for producing a cubic boron nitride polycrystal according to the present disclosure.
  • FIG. 3 illustrates another example of a method for producing a cubic boron nitride polycrystal according to the present disclosure. ⁇ 2020/174921 3 ⁇ (:171? 2020/001436
  • FIG. 1 A first figure.
  • FIG. 4 is a diagram for explaining another example of the method for producing a cubic boron nitride polycrystal according to the present disclosure.
  • FIG. 5 is a diagram for explaining a conventional example of a method for producing a cubic boron nitride polycrystal.
  • an object of the present invention is to provide a cubic boron nitride polycrystal that can have a long tool life even when used as a tool, especially in high-load machining of difficult-to-cut materials. To aim.
  • a cubic boron nitride polycrystal can have a long tool life when used as a tool, especially even under high load machining of difficult-to-cut materials.
  • a cubic boron nitride polycrystal of the present disclosure is a cubic boron nitride polycrystal containing 98.5 volume% or more of cubic boron nitride,
  • the dislocation density of the cubic boron nitride is greater than 8 ⁇ 10 15 / 2 , the cubic boron nitride polycrystal includes a plurality of crystal grains,
  • the cubic boron nitride polycrystal in which the median diameter 50 of the circle equivalent diameters of the plurality of crystal grains is not less than 0.1 and not more than 0.5.
  • a cubic boron nitride polycrystal body can have a long tool life when used as a tool, particularly even in high-load machining of difficult-to-cut materials.
  • the dislocation density is preferably 9 XI 0 15 / O 12 or more. to this ⁇ 2020/174921 4 ⁇ (:171? 2020 /001436
  • a method for producing a cubic boron nitride polycrystal according to the present disclosure is the above method for producing a cubic boron nitride polycrystal
  • the hexagonal boron nitride powder passes through the temperature and pressure within the stable region of the wurtzite boron nitride, 1 700 ° ⁇ As 2500 ° ⁇ following temperature and heated up to the pressure on 8_Rei 3 or more
  • the step of pressing
  • the stable region of the wurtzite boron nitride is a region that simultaneously satisfies the following formula 1 and formula 2 when the temperature is set to ( ° ⁇ , the pressure is ( ⁇ a), and the formula 1 is represented by: Ding + 1 1. 301
  • the plunge temperature of the wurtzite type boron nitride into the stable region is 500 ° or less
  • the step of applying heat and pressure includes the step of maintaining the temperature and pressure in the stable region of the wurtzite boron nitride for 10 minutes or more.
  • the cubic boron nitride polycrystal obtained by this manufacturing method can have a long tool life when used as a tool, especially even in high-load machining of difficult-to-cut materials.
  • the rush temperature is preferably 300° or less. according to this
  • the tool life using the obtained cubic boron nitride polycrystal is further improved.
  • the heating and pressurizing step includes a step of holding at a temperature and a pressure within the stable region of the wurtzite type boron nitride for 15 minutes or more. According to this, the life of a tool using the obtained cubic boron nitride polycrystal is further improved.
  • the life of a tool using the obtained cubic boron nitride polycrystal is further improved.
  • a cubic boron nitride polycrystal according to an embodiment of the present disclosure will be described.
  • the cubic boron nitride polycrystal of the present disclosure is a cubic boron nitride polycrystal containing cubic boron nitride in an amount of 98.5% by volume or more, and the dislocation density of the cubic boron nitride is 8 X 1 0 15 / 2 , the cubic boron nitride polycrystal contains a plurality of crystal grains, and the median diameter 50 of the circle-equivalent diameter of the plurality of crystal grains is not less than 0.1 and not more than 0.5111.
  • the cubic boron nitride polycrystal of the present disclosure is a sintered body, but since a sintered body is usually intended to include a binder, it is referred to as a "polycrystal" in the present disclosure. The term is used.
  • the cubic boron nitride polycrystal body of the present disclosure When used as a tool, it can have a long tool life even in high-load machining of difficult-to-cut materials. The reason for this is not clear, but it is presumed to be as follows (()) to (()).
  • the cubic boron nitride polycrystal of the present disclosure is a cubic boron nitride 98.5 volume.
  • the dislocation density of cubic boron nitride is higher than 8 x 10 15 / 2 .
  • the cubic boron nitride polycrystal has a relatively large number of lattice defects in the polycrystal and a large strain, so that the strength is improved. Therefore, the tool using the cubic boron nitride polycrystal can have a long tool life even in high-load machining of difficult-to-cut materials.
  • the cubic boron nitride polycrystal of the present disclosure has a median diameter of circular equivalent diameter of a plurality of crystal grains contained therein of 50 (hereinafter, also referred to as "grain size"). .1 or more and 0.5 or less.
  • grain size Conventionally, cubic boron nitride polycrystals were thought to have improved cutting performance because the smaller the grain size, the greater the strength. For this reason, the grain size of the crystal grains forming the cubic boron nitride polycrystal has been reduced (for example, the average grain size of 100 n However, due to this, the toughness tended to decrease.
  • the cubic boron nitride polycrystal of the present disclosure secures strength by increasing the dislocation density of cubic boron nitride, as described in (_
  • the tool using can have a long tool life even in high-load machining of difficult-to-cut materials.
  • the cubic boron nitride polycrystal of the present disclosure has a long tool life in high-load machining of difficult-to-cut materials, but the work material and the processing method are not limited to these. Not done.
  • the work material include a Dingyo alloy such as Dingyo 688 V and Cobalt chrome alloy.
  • processing methods include turning and milling.
  • the cubic boron nitride polycrystalline body of the present disclosure contains 98.5% by volume or more of cubic boron nitride.
  • the cubic boron nitride polycrystal has excellent hardness and excellent thermal stability and chemical stability.
  • the cubic boron nitride polycrystal is a cubic boron nitride within a range showing the effect of the present disclosure. ⁇ 2020/174921 7 ⁇ (:171? 2020/001436
  • compression type hexagonal boron nitride and wurtzite type boron nitride may be contained in a total amount of not more than 1.5% by volume.
  • compressed hexagonal boron nitride has a crystal structure similar to that of ordinary hexagonal boron nitride, and the interplanar spacing in the ⁇ axis direction is that of the regular hexagonal boron nitride ( ⁇ 0.33 3 less than n).
  • the cubic boron nitride polycrystal may contain an unavoidable impurity within a range that exhibits the effects of the present disclosure.
  • Inevitable impurities include, for example, hydrogen, oxygen, carbon, alkali metal elements (lithium (!_ ⁇ ), sodium (1 ⁇ 1 , And metal elements such as potassium ( ⁇ ) and alkaline earth metal elements (calcium (03), magnesium, etc.).
  • the content of the unavoidable impurities is preferably not more than 0.1% by volume.
  • the content of unavoidable impurities can be measured by secondary ion mass spectrometry (3).
  • the cubic boron nitride polycrystal does not substantially contain a binder, a sintering aid, a catalyst and the like. As a result, the strength and thermal diffusivity of the cubic boron nitride polycrystal are improved.
  • the content of cubic boron nitride in the cubic boron nitride polycrystal is preferably 98.5% by volume or more and 100% by volume or less, and more preferably 99% by volume or more and 100% by volume or less. preferable.
  • the total content of the compression type hexagonal boron nitride and the wurtzite type boron nitride in the cubic boron nitride polycrystal is 0% by volume or more! .5% by volume or less is preferable, 0% by volume or more and 1% by volume or less is more preferable, and 0% by volume is most preferable. That is, it is most preferable that the cubic boron nitride polycrystal does not contain either compression type hexagonal boron nitride or wurtzite type boron nitride.
  • the content of the compression type hexagonal boron nitride in the cubic boron nitride polycrystal is preferably 0 volume% or more and 1.5 volume% or less, more preferably 0 volume% or more and 1 volume% or less, and 0 volume% or less. % Is most preferred. That is, it is most preferable that the cubic boron nitride polycrystal does not contain compression type hexagonal boron nitride. ⁇ 2020/174921 8 ⁇ (:171? 2020 /001436
  • the content of wurtzite type boron nitride in the cubic boron nitride polycrystal is 0% by volume or more.
  • the cubic boron nitride polycrystal does not contain wurtzite type boron nitride.
  • the content (volume %) of cubic boron nitride, compression type hexagonal boron nitride and wurtzite type boron nitride in the cubic boron nitride polycrystal can be measured by an X-ray diffraction method.
  • the specific measuring method is as follows.
  • a cubic boron nitride polycrystal is cut with a diamond grindstone electrodeposition wire, and the cut surface is used as an observation surface.
  • X-ray diffraction method 0-20 method.
  • the content of the compression type hexagonal boron nitride can be obtained by calculating the value of peak strength/(peak strength tens peak strength ⁇ +peak strength ⁇ ). ⁇ 2020/174921 9 ⁇ (:171? 2020/001436
  • the content rate of boron nitride can be obtained by calculating the value of peak strength/(peak strength tens peak strength+peak strength ⁇ 3).
  • the cubic boron nitride content is obtained by calculating the values of peak strength ⁇ 3/ (peak strength tens peak strength + peak strength ⁇ ) compression type hexagonal boron nitride, wurtzite boron nitride and Since all cubic boron nitrides have the same electronic weight, the above X-ray peak intensity ratio can be regarded as the volume ratio in the cubic boron nitride polycrystal.
  • the dislocation density of the cubic boron nitride is greater than 8X 1 0 15 / ⁇ ! 2.
  • the cubic boron nitride polycrystal has relatively many lattice defects in the polycrystal and has a large strain, so that the strength is improved. Therefore, the tool using the cubic boron nitride polycrystal can have a long tool life even in high-load machining of difficult-to-cut materials.
  • Dislocation density 1 0 15 / Rei_1 more preferably 9X, 1. 0 X 1 0 16/2 or more is more preferable.
  • the upper limit of the dislocation density is not particularly limited, but from the viewpoint of manufacturing, 1.4 X 1 0 1 Can be That is, the dislocation density is preferably higher than 8 x 10 15 / 2 and not higher than 1.4 x 10 16 / ⁇ 12 and not less than 9 x 10 15 / ⁇ 12 ! 4 X 1 0 16 / ⁇ 12 or less is more preferable, and! .0 X 1 0 16 / ⁇ 12 or more! .4 X 1 0 16 / ⁇ 12 or less is more preferable ⁇
  • the dislocation density is calculated by the following procedure.
  • test piece made of a cubic boron nitride polycrystal is prepared.
  • the size of the test piece is 2.001111X2.00101 on the observation surface and 1.00101 on the thickness. Polish the observation surface of the test piece.
  • X-ray source Synchrotron radiation ⁇ 2020/174921 10 ⁇ (:171? 2020 /001436
  • Incident slit Width 5 ⁇ 1 ⁇ 1 Height ⁇ 0.5 ⁇ 1 111
  • Double slit Double slit (width 3 ⁇ ! ⁇ ! X height ⁇ 0.5 ⁇ ! ⁇ !)
  • Measurement condition The number of measurement points should be 9 or more in the half-width.
  • the peak top strength shall be 2,000 0.003 or more. Since the bottom of the peak is also used for the analysis, the measurement range should be about 10 times the full width at half maximum.
  • the line profile obtained by the above X-ray diffraction measurement has a shape that includes both the true spread due to the physical quantity such as non-uniform strain of the sample and the spread due to the apparatus.
  • the instrument-induced components are removed from the measured line profile to obtain a true line profile.
  • the true line profile is obtained by fitting the obtained line profile and the device-induced line profile by a pseudo ⁇ function and subtracting the device-induced line profile.
  • a standard sample for removing the diffraction line spread due to the equipment ! _ 3 and 6 were used.
  • synchrotron radiation with high parallelism is used, the diffraction line spread due to the device can be regarded as ⁇ .
  • ⁇ ⁇ [1-9 ( ⁇ + 2 1 2 + 1 ⁇ 2 1 2 )Pa +1 ⁇ 2 + 1 2 ) 2 ] (II) 0
  • the coefficients relating to the contrast factor ⁇ _ and the contrast factor of the screw dislocation and the edge dislocation are calculated by using the calculation code 8 1 ⁇ 1 ⁇ , and the slip system is ⁇ 1 1 0> ⁇ 1 1 1 ⁇ , elastic stiff 4409 a s ⁇ 12 is calculated as 1.90 3 and ⁇ 44 is calculated as 4.83 ⁇ 3.
  • the contrast factor ⁇ _ is ⁇ .203 for the screw dislocation and ⁇ 0.21 for the edge dislocation.
  • the coefficient 9 for the contrast factor is 1.65 for screw dislocations and 0.58 for edge dislocations.
  • the screw dislocation ratio is fixed at 0.5 and the edge dislocation ratio is fixed at 0.5.
  • the median diameter d 50 (hereinafter, also referred to as “median diameter d 50 ”) of the circle-equivalent diameter of a plurality of crystal grains contained in the cubic boron nitride polycrystal of the present disclosure is 0.1 Mm or more and 0.5 or more. It is less than or equal to Mm.
  • cubic cubic boron nitride polycrystals were considered to have higher strength and smaller cutting performance as the grain size was smaller. For this reason, the grain size of the crystal grains forming the cubic boron nitride polycrystal was reduced (for example, the average grain size was less than 100 nm), but this tended to reduce toughness.
  • the cubic boron nitride polycrystal of the present disclosure as described in (N) above, strength is secured by increasing the dislocation density of cubic boron nitride. Can be made larger than before. Therefore, the cubic boron nitride polycrystal of the present disclosure has improved toughness and can have excellent crack propagation resistance. Therefore, the tool using the cubic boron nitride polycrystal can have a long tool life even in high-load machining of difficult-to-cut materials.
  • the equivalent median diameter 50 is obtained by measuring the median diameters 50 of multiple crystal grains at each of the arbitrarily selected 5 measurement points and calculating the average value of these. Means the value.
  • the portion of the cubic boron nitride polycrystal is cut with a diamond grindstone electrodeposition wire or the like, and the cut cross section is polished. , Set 5 measurement points arbitrarily on the polished surface.
  • the cubic boron nitride polycrystal is cut with a diamond grindstone electrodeposition wire or the like so that the measurement points are exposed, and the cut surface is polished.
  • 3M IV! image is obtained by observing the measurement points on the polished surface using 3M IV! (“3 1 1//1-7500” (product name) manufactured by JEOL Ltd.). ..
  • the size of the measurement field of view is 1 2 15 and the observation magnification is 10000.
  • the image processing software 0 « _ ⁇ ⁇ ⁇ “. 7. 4. Using 5), calculate the distribution of equivalent circle diameters for each crystal grain.
  • the median diameter 50 is calculated with the entire measurement visual field as the denominator. Calculate the median diameter 50 from the distribution of equivalent circle diameters of crystal grains.
  • the cubic boron nitride polycrystal of the present disclosure is suitable for use in cutting tools, abrasion resistant tools, grinding tools, and the like.
  • the cutting tool, the wear-resistant tool, and the grinding tool using the cubic boron nitride polycrystal of the present disclosure may each be entirely composed of the cubic boron nitride polycrystal. ⁇ 2020/174921 14 ⁇ (: 171? 2020 /001436
  • a part thereof may be composed of cubic boron nitride polycrystal.
  • a coating film may be formed on the surface of each tool.
  • Examples of cutting tools include drills, end mills, cutting edge exchangeable cutting tips for drills, cutting edge exchangeable cutting tips for end mills, cutting edge exchangeable cutting tips for milling, cutting edge exchangeable cutting tips for turning, metal saws, teeth. Mention may be made of cutting tools, reamers, dups, cutting bits, etc.
  • Examples of the wear resistant tool include a die, a scraper, a scribing wheel, and a dresser.
  • a grinding wheel can be used as the grinding tool.
  • FIGS. 1 to 5 A method for manufacturing a cubic boron nitride polycrystal according to the present disclosure will be described with reference to FIGS. 1 to 5.
  • Figure 1 is a pressure-temperature phase diagram for boron nitride.
  • 2 to 4 are diagrams for explaining a method for manufacturing a cubic boron nitride polycrystal body according to the present disclosure.
  • FIG. 5 is a diagram for explaining a conventional example of a method for producing a cubic boron nitride polycrystal.
  • the method for producing a cubic boron nitride polycrystal according to the present disclosure is the method for producing a cubic boron nitride polycrystal according to the first embodiment.
  • a method for producing a cubic boron nitride polycrystal according to the present disclosure includes a step of preparing a hexagonal boron nitride powder (hereinafter, also referred to as a “preparing step”), and a step of preparing the hexagonal boron nitride powder from wurtzite boron nitride.
  • the stable region of wurtzite boron nitride is a region that simultaneously satisfies the following formula 1 and formula 2 when the temperature is set to ( ° ⁇ ) and the pressure is set to (09 a). -0 ⁇ 0 0 3 7 + 1 1 .3 0 1
  • the plunge temperature of the wurtzite type boron nitride into the stable region is 500 ° or less, and in the heating and pressing process, the temperature and pressure in the stable region of the wurtzite type boron nitride is 10 min or more.
  • the step of holding is included.
  • boron nitride includes hexagonal boron nitride which is a stable phase at room temperature and normal pressure, cubic boron nitride which is a stable phase at high temperature and high pressure, and hexagonal boron nitride.
  • hexagonal boron nitride There are three phases of wurtzite boron nitride, which are metastable phases during the dislocation to cubic boron nitride.
  • each phase can be represented by a linear function.
  • the temperature and pressure in the stable region of each phase can be shown by using a linear function.
  • Min 1 ⁇ ! Stable region Is defined as the temperature and pressure that simultaneously satisfy the following formula 1 and formula 2 when the temperature is (° ⁇ ) and the pressure is ( ⁇ 3).
  • the temperature and pressure in the stable region of hexagonal boron nitride (in Fig. 1, referred to as "11M 1 ⁇ 1 stable region"), the temperature is exactly (° ⁇ ),
  • the pressure is ( ⁇ 3)
  • it is defined as the temperature and pressure that simultaneously satisfy the following equation 8 and the following equation, or the temperature and pressure that simultaneously satisfy the following equation ⁇ 3 and the following equation 0.
  • I will write it as " ⁇ Mi 1 ⁇ 1 stable region". ) Is defined as the temperature and pressure that simultaneously satisfy the following formula port and the following formula when the temperature is (° ⁇ ) and the pressure is (° 9 a).
  • the temperature in the stable region of cubic boron nitride hereinafter, also referred to as “target temperature”
  • pressure hereinafter, “When heating and pressurizing to the target pressure, first increase the pressure to the target pressure (about 80 3 in Fig. 5) (arrow 1 in Fig. 5), and then change the temperature to the target temperature (Fig. In Fig. 5, the temperature is raised to approximately 1900° ⁇ (arrow 2 in Fig. 5).
  • the heating and pressurizing operation is simple in the path of Fig. 5 because heating and pressurization are each performed once. , Which was previously adopted.
  • the cubic boron nitride polycrystal content in the cubic boron nitride polycrystal means that the cubic boron nitride polycrystal, together with the cubic boron nitride, contains hexagonal boron nitride and/or wurtzite boron nitride. When included, it means the content of cubic boron nitride when the total of the contents of cubic boron nitride, hexagonal boron nitride and wurtzite boron nitride is used as the denominator.
  • the plunge temperature of the wurtzite boron nitride into the stable region is related to the dislocation density of the cubic boron nitride.
  • the strength of the obtained cubic boron nitride polycrystal was affected.
  • the inventors of the present invention consider the above situation and the effect of the grain size of a plurality of crystal grains contained in the cubic boron nitride polycrystal on the toughness, while considering the cubic boron nitride polycrystal.
  • the route of pressure and temperature in the manufacturing process was thoroughly studied.
  • the present inventors have found a heating and pressurizing condition capable of obtaining a cubic boron nitride polycrystal that can have a long tool life even when processing difficult-to-cut materials.
  • FIGS. 2 to 4 will be described below. 2 to 4, the arrow indicates the heating/pressurizing path. A circle at the tip of the arrow indicates that the temperature and pressure are maintained for a certain period of time.
  • the routes shown in FIGS. 2 to 4 are examples, and the present invention is not limited to these.
  • a hexagonal boron nitride powder is prepared as a raw material for the cubic boron nitride polycrystal.
  • the hexagonal boron nitride powder has a purity (hexagonal boron nitride content) of 98.5% or more. ⁇ 2020/174921 18 ⁇ (:171? 2020 /001436
  • the particle size of the hexagonal boron nitride powder is not particularly limited, but can be, for example, not less than 0.1 Mm and not more than 10 m.
  • the hexagonal boron nitride powder is passed through the temperature and pressure in the stable region of the wurtzite type boron nitride to a temperature of 1700 ° C or higher and 2500 ° C or lower (hereinafter also referred to as “achieved temperature”). ) And, and heating and pressurization up to a pressure of 8 GPa or more (hereinafter also referred to as “attainment pressure”) (arrows A 1, A 2 and A 3 in FIG. 2, arrows B 1, B 2 in FIG. 3). , B3 and B4, arrows C1, C2, C3 and C4 in Figure 4).
  • the plunge temperature of wurtzite boron nitride into the stable region is 500 °C or less.
  • the heating/pressurizing step includes a step of maintaining the temperature and pressure in the stable region of the wurtzite boron nitride for 10 minutes or more (a 1 in FIG. 2 and b in FIG. 3).
  • the rush temperature of the wurtzite boron nitride into the stable region means the temperature at the time when the wurtzite boron nitride reaches the stable region for the first time in the heating and pressing step.
  • the plunge temperature of the wurtzite boron nitride into the stable region was 5
  • the hexagonal boron nitride powder is converted into wurtzite type boron nitride in an environment where atomic diffusion does not easily occur, and then converted to cubic boron nitride. Therefore, the obtained cubic boron nitride polycrystal has a relatively large number of lattice defects in the polycrystalline body, and the cubic boron nitride has a large dislocation density and a large strain, resulting in improved strength. doing. Therefore, a tool using the cubic boron nitride polycrystal can have a long tool life even in high-load machining of difficult-to-cut materials. ⁇ 2020/174921 19 ⁇ (:171? 2020/001436
  • the plunge temperature of the wurtzite boron nitride into the stable region is 300 ° C or less
  • Inrush temperature to the stable region of the wurtzite boron nitride is preferably 1 0 ° ⁇ As 5 00 ° ⁇ less, more preferably 1 0 ° ⁇ As 300 ° ⁇ below 1 0 ° ⁇ than the 1 00 ° ⁇ less Is more preferable.
  • the heating and pressurizing step is performed at a temperature and a pressure within the stable region of the wurtzite boron nitride.
  • the step of holding for 10 minutes or more since the retention time of the wurtzite boron nitride in the stable region is long, the conversion rate from hexagonal boron nitride to wurtzite boron nitride is improved, and as a result, the conversion rate to cubic boron nitride is also increased. improves. Therefore, the obtained cubic boron nitride polycrystal has an increased content of cubic boron nitride and is less likely to be damaged during processing. Therefore, a tool using the cubic boron nitride polycrystal can have a long tool life even in high-load machining of difficult-to-cut materials.
  • the holding time of the wurtzite boron nitride at the temperature and pressure in the stable region is preferably 15 minutes or longer, more preferably 30 minutes or longer. From the viewpoint of production, the upper limit of the holding time is preferably 60 minutes.
  • the holding time is preferably 10 minutes or more and 60 minutes or less, more preferably 15 minutes or more and 60 minutes or less, and further preferably 30 minutes or more and 60 minutes or less.
  • heating and pressurizing process when the temperature is set to () and the pressure is set to ( ⁇ 3), the temperature and the pressure in the area satisfying the following formula 1, formula 2 and formula 3 at the same time are 10 minutes. It is preferable to include a step of holding the above (hereinafter also referred to as “heating and pressing step”).
  • a region that simultaneously satisfies the above formulas 1, 2 and 3 is defined as a stable region of wurtzite boron nitride and a stable region of hexagonal boron nitride and a stable region of wurtzite boron nitride. ⁇ 2020/174921 20 ⁇ (:171? 2020 /001436
  • the obtained cubic boron nitride polycrystal has a large number of lattice defects in the polycrystal and has a large strain, so that the strength is further improved. Therefore, the tool using the cubic boron nitride polycrystal can have a longer tool life even in high-load machining of difficult-to-cut materials.
  • the holding time at the temperature and the pressure in the region simultaneously satisfying the above formulas 1, 2 and 3 is more preferably 15 minutes or more, further preferably 20 minutes or more. From the viewpoint of production, the upper limit of the holding time is preferably 60 minutes.
  • the holding time is preferably 10 minutes or more and 60 minutes or less, more preferably 15 minutes or more and 60 minutes or less, and further preferably 20 minutes or more and 60 minutes or less.
  • the heating/pressurizing step includes the step of holding for 10 minutes or more at the temperature and pressure in the region simultaneously satisfying the above formulas 1, 2 and 3, the heating/pressurizing step is followed by the following formula 2 And a step of holding at a temperature and pressure in a region satisfying the following formula 4 for 1 minute or more (hereinafter, also referred to as “heating and pressing step”).
  • Equation 2 9 £-0. 0 8 5 1 + 1 1 7
  • the conversion rate from hexagonal boron nitride to wurtzite boron nitride is further improved, and as a result, the conversion rate to cubic boron nitride is also improved.
  • the obtained cubic boron nitride polycrystal has an increased content of cubic boron nitride and is less likely to have defects during processing. Therefore, a tool using the cubic boron nitride polycrystal can have a long tool life even in high-load machining of difficult-to-cut materials.
  • the holding time at the temperature and pressure in the region satisfying the above formulas 2 and 4 is more preferably 10 minutes or more, further preferably 15 minutes or more. From the viewpoint of manufacturing, the upper limit of the holding time is preferably 60 minutes.
  • the holding time is preferably 1 minute or more and 60 minutes or less, more preferably 10 minutes or more and 60 minutes or less, and further preferably 15 minutes or more and 60 minutes or less.
  • heating and pressing step only the above heating and pressing step may be performed, or the above heating and pressing step may be performed after the above heating and pressing step. Also, ⁇ 2020/174921 21 ⁇ (:171? 2020 /001436
  • the heating/pressurizing step may be a step of holding for 10 minutes or more in a region satisfying the above formulas 2 and 4.
  • the ultimate pressure in the heating and pressurizing step is 8°C or higher, preferably 103°C or higher, and more preferably 13°C 3 or higher.
  • the upper limit of the ultimate pressure is not particularly limited, but may be, for example, 15° 3.
  • the ultimate pressure in the heating and pressurizing step is preferably 80 3 or more and 150 9 a or less, more preferably 10° 3 or more and 15 5 3 or less, and further preferably 13 3 3 or more 15 5 3 or less
  • heating and pressurizing step in the route of Figs. 2 to 4, heating is performed, then pressure is applied, and further heating is performed, but the heating and pressurizing route is not limited to this.
  • the heating and pressurizing route is such that the entry temperature of the wurtzite boron nitride into the stable region is 500 ° C or lower, and the temperature and pressure in the stable region of the wurtzite boron nitride can be maintained for 10 minutes or more.
  • heating and pressurization may be performed simultaneously.
  • a cubic boron nitride polycrystal can be obtained by subjecting the hexagonal boron nitride powder to the heating and pressing step.
  • a cubic boron nitride polycrystal body obtained by hot pressing step 1 7 0 0 ° ⁇ As 2 5 0 0 ° ⁇ temperatures below (hereinafter, "the final sintering temperature "and also referred.), and, 8 0 3 or more pressure (hereinafter, a step of holding" final sintered pressure "both referred.) 3 minutes or 6 0 minutes following conditions.
  • the obtained cubic boron nitride polycrystal has a large cubic boron nitride content, and a longer tool life can be achieved.
  • the final sintering temperature is preferably not less than 1900° and not more than 2400°.
  • the final sintering pressure is preferably 8°3 or more and 15°3 or less, more preferably 10°3 or more and 15°3 or less.
  • the holding time in the final sintering step is preferably 10 minutes or more and 20 minutes or less. ⁇ 2020/174921 22 ⁇ (:171? 2020 /001436
  • the temperature is raised from the starting point 3 to a predetermined temperature of 500 ° ⁇ or less (about 250 ° ⁇ in Fig. 2) (arrow 8 1), and then the wurtzite boron nitride is maintained while maintaining the temperature.
  • the pressure in the stable region (approx. 1309 a in Fig. 2) is increased (arrow 8), and it is maintained for 10 minutes or longer at that temperature (approx. 250° ⁇ and pressure (approx. 1309 a)) (Fig. 2). 3 1).
  • the temperature 1 700 ° ⁇ As 2500 ° ⁇ below (the temperature was raised to about 2000 ° ⁇ in Figure 2 (arrow 3) pressure, the at a temperature (about 2000 ° ⁇ and pressure (about 1 30 3), hold 3 minutes to 60 minutes or less (3 of Fig. 2 2) in.
  • Figure 2 the heating and pressing step, arrows 1, 2 and 3, And And the final sintering step is 32.
  • the entry temperature of the wurtzite type boron nitride into the stable region is 500° ⁇ or less (about 250 ° ⁇ .
  • the hexagonal boron nitride powder is in an environment where atomic diffusion does not easily occur. Therefore, it is converted into wurtzite type boron nitride, and then converted into cubic boron nitride.. Therefore, the obtained cubic boron nitride polycrystal has relatively many lattice defects in the polycrystal.
  • the cubic boron nitride has a large dislocation density and a large strain, the strength is improved, so that a tool using the cubic boron nitride polycrystal can be used even in high-load machining of difficult-to-cut materials. Can have long tool life.
  • the temperature and pressure in the stable region of the wurtzite boron nitride are maintained for 10 minutes or more.
  • the retention time of the wurtzite boron nitride in the stable region is long, the conversion rate from hexagonal boron nitride to wurtzite boron nitride is improved, and as a result, the conversion rate to cubic boron nitride is also increased. improves. Therefore, the cubic boron nitride polycrystal obtained has an increased content of cubic boron nitride, and is less likely to be damaged during processing. Therefore, a tool using the cubic boron nitride polycrystal can have a long tool life even in high-load machining of difficult-to-cut materials.
  • the cubic boron nitride polycrystal obtained by the heating and pressurizing step is ⁇ 2020/174921 23 ⁇ (:171? 2020/001436
  • the obtained cubic boron nitride polycrystal has a large cubic boron nitride content and can have a longer tool life.
  • the temperature is raised from the starting point 3 to a predetermined temperature of 500 ° ⁇ or less (about 250 ° ⁇ in Fig. 3) (arrow arrow 1), and then while maintaining the temperature, the following equation 1,
  • the pressure in the region that simultaneously satisfies the following formulas 2 and 3 is increased (arrow 2), and the temperature (about 250° ⁇ and the pressure (about 10.40a) is measured.
  • step 3 hold for 10 minutes or more (1 in Fig. 3).
  • the entry temperature of the wurtzite type boron nitride into the stable region is 500° ⁇ or less (about 250 ° ⁇ .
  • the hexagonal boron nitride powder is in an environment where atomic diffusion does not easily occur. Therefore, it is converted into wurtzite type boron nitride, and then converted into cubic boron nitride.. Therefore, the obtained cubic boron nitride polycrystal has relatively many lattice defects in the polycrystal.
  • the path of Fig. 3 includes a step of holding the temperature and pressure in a region that simultaneously satisfies the above formula 1, formula 2 and formula 3 for 10 minutes or more. That is, the path of FIG. 3 is more stable than the path of FIG. 2 within the stable region of wurtzite boron nitride and at a temperature and pressure closer to the stable region of hexagonal boron nitride (i.e., of wurtzite boron nitride). The temperature and pressure in the vicinity of the boundary between the stable region and the stable region of hexagonal boron nitride are maintained for 10 minutes or more. For this reason, lattice defects are more likely to occur than in the route of FIG.
  • the cubic boron nitride polycrystal obtained by the route of FIG. 3 becomes the cubic boron nitride polycrystal obtained by the route of FIG. Compared with this, it is considered that the polycrystalline body has more lattice defects and the strain is large, so that the strength is further improved. Therefore, the tool using the cubic boron nitride polycrystal obtained by the route of FIG. 3 can have a longer tool life even in high-load machining of difficult-to-cut materials.
  • the cubic boron nitride polycrystal obtained by the heating and pressurizing step was processed under the conditions of 1 700 °C or higher and 2500 °C or lower and pressure conditions of 8 GPa or higher. Hold for 60 minutes or more.
  • the obtained cubic boron nitride polycrystal has a large cubic boron nitride content and can have a longer tool life.
  • the temperature is raised from the starting point S to a predetermined temperature of 500 °C or less (about 250 ° C in Fig. 4) (arrow C 1), and then while maintaining the temperature, the following equation 1,
  • the pressure is raised to a pressure (about 10.4 GPa in Fig. 4) in the region that simultaneously satisfies the following formulas 2 and 3, and the temperature (about 250°C) and the pressure (about 10. Hold for 10 minutes or more at 4 GP a) (c 1 in Figure 3).
  • Equation 1 P3_. 0037 T+ 1 1. 301
  • Equation 3 P £-0. 0037 T+ 1 1.375.
  • Equation 2 P£-0. 085 T+ 1 1 7
  • Equation 4 P>-0. 0037 T+ 1 1.375.
  • the temperature was raised to 1 700 ° C or higher and 2500 °C or lower (about 2000 °C in Fig. 4) (arrow C4), Hold at the temperature (about 2000°C) and the pressure (about 13 GPa) for 3 minutes or more and 60 minutes or less (c 3 in Fig. 4).
  • the heating and pressing step is indicated by arrows C 1, C 2, 0 3 and 04, and c 1 and c 2, and the final sintering step is indicated by c 3.
  • the entry temperature of the wurtzite boron nitride into the stable region is 500°C or lower (about 250 ° C).
  • the hexagonal boron nitride powder is converted to wurtzite type boron nitride in an environment where atomic diffusion does not easily occur, and then converted to cubic boron nitride.
  • the obtained cubic boron nitride polycrystal has a relatively large number of lattice defects in the polycrystal, and the cubic boron nitride has a large dislocation density and a large strain. There is. Therefore, a tool using the cubic boron nitride polycrystal can have a long tool life even in high-load machining of difficult-to-cut materials.
  • the path of Fig. 4 includes a step of maintaining the temperature and the pressure in the region where the above formula 1, the above formula 2 and the above formula 3 are simultaneously satisfied for 10 minutes or more. That is, the route of FIG. 4 is more stable than the route of FIG. 2 in the stable region of wurtzite boron nitride and at a temperature and pressure closer to the stable region of hexagonal boron nitride (ie, in the wurtzite boron nitride). The temperature and pressure in the vicinity of the boundary between the stable region and the stable region of hexagonal boron nitride are maintained for 10 minutes or more. Therefore, in the route of FIG.
  • the tool using the cubic boron nitride polycrystal obtained through the route of FIG. 4 can have a longer tool life even in high-load machining of difficult-to-cut materials.
  • Equation 2 9 £-0.08 5 1 + 1 1 7
  • the conversion rate from hexagonal boron nitride to wurtzite boron nitride is further improved as compared with the route of Fig. 3, and as a result, the conversion rate to cubic boron nitride is increased. Also improves. Therefore, the cubic boron nitride polycrystal obtained by the route of FIG. 4 has a higher content of cubic boron nitride nitride than the cubic boron nitride polycrystal obtained by the route of FIG. , It is unlikely that a defect will occur during processing. Therefore, the tool using the cubic boron nitride polycrystal can have a longer tool life even in high-load machining of difficult-to-cut materials.
  • the cubic boron nitride polycrystal obtained by the heating and pressurizing step is treated at a temperature of 1700 ° ° or more and 2500 ° ° or less, and 803 or more. Hold for 3 to 60 minutes under pressure.
  • the cubic boron nitride polycrystal obtained has a high cubic boron nitride content, and can achieve a longer tool life.
  • Example 1 the production conditions of the cubic boron nitride polycrystal, the composition of the obtained cubic boron nitride nitride polycrystal (composition, median diameter of crystal grains, dislocation density), and the cubic boron nitride polycrystal
  • composition, median diameter of crystal grains, dislocation density Composition, median diameter of crystal grains, dislocation density
  • the cubic boron nitride polycrystals of Sample 1 to Sample 9 were manufactured according to the following procedure.
  • Hexagonal boron nitride powder (“Denka Boron Nitride” (trade name) manufactured by Denka Co., Ltd., particle size: 50) was prepared.
  • the above hexagonal boron nitride powder was put in a molybden capsule and placed in an ultrahigh pressure and high temperature generator.
  • the high temperature and high pressure treatment at the "attainment pressure” and “holding time” corresponds to the final sintering process.
  • the content of cubic boron nitride in the cubic boron nitride polycrystal obtained above was measured by an X-ray diffraction method. Since the specific method of the X-ray diffraction method is as shown in the first embodiment, the description thereof will not be repeated. The results are shown in the “ ⁇ Mi content” column of Table 1. ⁇ 2020/174 921 29 ⁇ (: 171? 2020 /001436
  • the dislocation density of cubic boron nitride in the cubic boron nitride polycrystal obtained above was corrected by the line profile obtained by X-ray diffraction measurement. 1 1 1 1 Method and modified 13 ““6 ⁇ 8 ⁇ 6 3 0 11 method was used for analysis. The specific calculation method of the dislocation density is as shown in the first embodiment. The results are shown in the “Dislocation density” column of Table 1.
  • the cubic boron nitride polycrystal obtained above was cut by laser and finished, and the insert model number 1 ⁇ 1 11 - ⁇ ⁇ 08 1 2 0 4 0 8 (Sumitomo Electric Ehard Metal Co., Ltd.) A cutting tool was produced. Using the cutting tool obtained, intermittently cut a 6-88-round 4 round bar (0 2 X 0 X 10 1, with one V-shaped slit) under the following cutting conditions to extend the tool life. evaluated. Note that the 6 I 4 round bar that is the work material is a difficult-to-cut material.
  • Feed amount ⁇ .01111/blade ⁇ 2020/174921 30 ⁇ (: 171-1? 2020 /001436
  • the above cutting conditions correspond to high load machining of difficult-to-cut materials.
  • the cubic boron nitride polycrystals from 1-1 to Sample 1_3 all contained 98.5% by volume or more of cubic boron nitride, and the dislocation density of cubic boron nitride was 8 1 It is larger, and the median diameter 50 of the crystal grains is not less than 0.1 and not more than 0.5, which corresponds to the example. It was confirmed that the tools using the cubic boron nitride polycrystals of Sample 1 _ 1 to Sample 1 _ 3 have a long tool life even in the high load machining of difficult-to-cut materials.
  • Sample 1 _ 1 was longer than Sample 1 _ 3. This is because Sample 1-1 has a longer holding time at the ultimate temperature and ultimate pressure (that is, in the stable region of wurtzite boron nitride) in the second stage than Sample 1-3, so that it is a hexagonal crystal.
  • the conversion rate from boron nitride to wurtzite type boron nitride was further improved, and as a result, the conversion rate to cubic boron nitride was improved.
  • the cubic boron nitride polycrystals from 2-1 to Sample 2 _ 3 all contain cubic boron nitride in an amount of 98.5% by volume or more, and the dislocation density of cubic boron nitride is 8 1 It is larger, and the median diameter 50 of the crystal grains is not less than 0.1 and not more than 0.5, which corresponds to the example. It was confirmed that the tools using the cubic boron nitride polycrystals of Samples 2 _ 1 to Sample 2 _ 3 have a long tool life even in high load machining of difficult-to-cut materials. ⁇ 2020/174921 33 ⁇ (:171? 2020/001436
  • Sample 2-1 was longer than Sample 2-3. This is because Sample 2-1 has a longer holding time at the ultimate temperature and ultimate pressure (that is, within the stable region of wurtzite type boron nitride) in the third stage than Sample 2-3, so hexagonal nitriding It is considered that the conversion rate from boron to wurtzite type boron nitride was further improved, and as a result, the conversion rate to cubic boron nitride was higher than that of sample 2 _ 3, and the content of cubic boron nitride was high.
  • Sample 3_1 to Sample 3_3 all correspond to the examples.
  • Cubic boron nitride polycrystal 1 Sample 3 _ 3 are both cubic boron nitride 9 8 5 comprises vol% or more, the dislocation density is 81 cubic boron nitride 0 1 5/2 It is larger, and the median diameter 50 of the crystal grains is not less than 0.1 and not more than 0.5, which corresponds to the example. It was confirmed that the tools using the cubic boron nitride polycrystals of Samples 3 _ 1 to Sample 3 _ 3 have a long tool life even under high load machining of difficult-to-cut materials.
  • Sample 3-1 was longer than Sample 3-3. This is because Sample 3-1, compared to Sample 3-3, ⁇ 2020/174921 34 ⁇ (: 171? 2020 /001436
  • Cubic boron nitride polycrystal sample 4 and sample 7 are both comprise cubic boron nitride 9 8.5 body volume% or more, the dislocation density of the cubic boron nitride is greater than 8 X 1 0 1 5/2 , And the median diameter 50 of the crystal grains is not less than 0.1 and not more than 0.5, which corresponds to the example. It was confirmed that the tools using the cubic boron nitride polycrystals of Sample 4 and Sample 7 have a long tool life even under high load machining of difficult-to-cut materials.
  • Sample 4 has a higher pressure in the final sintering step and has a higher cubic boron nitride content than Sample 7.
  • the manufacturing methods of Samples 5 and 6 both correspond to comparative examples, in which the inrush temperature of wurtzite boron nitride into the stable region exceeds 500°C.
  • the cubic boron nitride polycrystals of Sample 5 and Sample 6 each have a dislocation density of cubic boron nitride of 8 ⁇ 10 15 / ⁇ 12 or less, and thus correspond to Comparative Examples.
  • the tool using the cubic boron nitride polycrystals of Sample 5 and Sample 6 had a short tool life.
  • the manufacturing method of Sample 8 does not include the step of maintaining the temperature and pressure in the stable region of the wurtzite boron nitride for 10 minutes or more, and corresponds to the comparative example.
  • the cubic boron nitride polycrystal of Sample 8 has a cubic boron nitride content of 98.3 volume% and is a comparative example.
  • the tool using the cubic boron nitride polycrystal of sample 8 has a long tool life. ⁇ 2020/174 921 35 ⁇ (: 171? 2020 /001436
  • the manufacturing method of Sample 9 does not include the step of maintaining the temperature and pressure in the stable region of the wurtzite type boron nitride for 10 minutes or more, and corresponds to the comparative example.
  • the cubic boron nitride polycrystal of Sample 9 has a cubic boron nitride content of 98.2% by volume and corresponds to the comparative example.
  • the tool using the cubic boron nitride polycrystal of Sample 9 had a short tool life.
  • the manufacturing method of Sample 9 does not include the step of holding for 10 minutes or more at the temperature and pressure in the stable region of wurtzite boron nitride, so that the conversion rate from hexagonal boron nitride to wurtzite boron nitride is high. It is thought that this is because the conversion rate to cubic boron nitride is low, resulting in a low cubic boron nitride content in the obtained cubic boron nitride polycrystal.
  • sample 9 was shorter than that of sample 4 because the retention time of the wurtzite type boron nitride in the stable region was shorter, resulting in a lower conversion rate to cubic boron nitride nitride and the obtained cubic It is considered that the content of cubic boron nitride in the cubic boron nitride polycrystal became smaller, and as a result, the cubic boron nitride polycrystal of Sample 9 had a shorter tool life than Sample 4.
  • Example 2 the manufacturing conditions of the cubic boron nitride polycrystal, the composition of the obtained cubic boron nitride nitride polycrystal (composition, median diameter of crystal grains, dislocation density), and the cubic boron nitride polycrystal
  • composition, median diameter of crystal grains, dislocation density Composition, median diameter of crystal grains, dislocation density
  • Hexagonal boron nitride powder (“Denka Boron Nitride” (trade name) manufactured by Denka Co., Ltd., particle size: 50) was prepared.
  • the above hexagonal boron nitride powder was put in a molybden capsule and placed in an ultrahigh pressure and high temperature generator.
  • the median diameter 50 of the circular equivalent diameters was measured. Since the specific method is as shown in the first embodiment, the description thereof will not be repeated. The results are shown in the “Median diameter (50)” column of Table 2.
  • the cubic boron nitride polycrystal obtained above was cut by laser and finished, and the insert model number A cutting tool manufactured by Sumitomo Electric Hardmetal Co., Ltd. was manufactured. Using the cutting tool obtained, under the following cutting conditions, gray iron ⁇ 300 block material
  • the above cutting conditions correspond to high-load machining of ferrous materials.
  • the manufacturing method of Sample 10 has a holding time of less than 3 minutes (2 minutes) in the third stage (final sintering step), and corresponds to the comparative example.
  • the cubic boron nitride polycrystal of Sample 10 has a median particle size of 50 of less than 0. 1 (0. 08), which corresponds to the comparative example.
  • the tool using the cubic boron nitride polycrystal of Sample 10 had a short tool life. This is presumably because in Sample 10, the holding time in the final sintering step was short, grain growth became insufficient, and the median diameter 50 of the crystal grains became small.
  • the manufacturing methods of Sample 11 and Sample 12 both correspond to Examples.
  • the cubic boron nitride polycrystals of Sample 11 and Sample 12 each contained cubic boron nitride of 98.5% by volume or more, and the dislocation density of cubic boron nitride was 8 1
  • the median diameter 50 of the crystal grains is larger and is greater than or equal to 0.1 and less than or equal to 0.5, which corresponds to the example. It was confirmed that the tools using the cubic boron nitride polycrystals of Sample 11 and Sample 12 have a long tool life even under high load machining of iron-based materials.
  • the manufacturing method of Sample 13 has a holding time of more than 60 minutes (70 minutes) in the third stage (final sintering step), and corresponds to the comparative example.
  • the cubic boron nitride polycrystal of Sample 13 has a median particle size of 50 of more than 0.5 (0.59), which corresponds to the comparative example.
  • the tool using the cubic boron nitride polycrystal of Sample 13 had a short tool life. This is probably because Sample 13 had a longer holding time in the final sintering step, so grain growth proceeded excessively and the median diameter 50 of the crystal grains increased.
  • Specimen 4 has a manufacturing method of 3rd stage (final sintering step) temperature of 1700° ⁇ (1650° ⁇ ), which corresponds to Comparative Example.
  • the crystalline body has a median particle diameter of 50 of less than 0. 1 (0. 09), which corresponds to the comparative example.
  • the tool using the cubic boron nitride polycrystal of Sample 14 had a short tool life. This is probably because in Sample 14, the temperature of the final sintering step was low, so grain growth became insufficient and the median diameter 50 of the crystal grains became small.
  • the manufacturing method of Sample 1 5 the temperature is 2 5 0 0 ° ⁇ than the third stage (the final sintering step) (a 2 5 5 0 ° ⁇ corresponds to a comparative example.
  • the manufacturing method of Sample 1 6 is a rush temperature to the stable region of the wurtzite boron nitride exceeded a 5 0 0 ° ⁇ (1 0 0 0 ° ⁇ ) corresponds to a comparative example.
  • the cubic boron nitride polycrystal of Sample 16 has a dislocation density of 8 x 1 of cubic boron nitride. Below (6. And corresponds to the comparative example.
  • the tool using the cubic boron nitride polycrystal of Sample 16 had a short tool life.

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Abstract

La présente invention concerne du nitrure de bore cubique polycristallin qui contient au moins 98,5 % en volume de nitrure de bore cubique, la densité de dislocation du nitrure de bore cubique étant supérieure à 8×1015/m2, le nitrure de bore cubique polycristallin comprenant de multiples grains cristallins, et le diamètre médian d50 des diamètres de cercle équivalent des multiples grains cristallins étant de 0,1 à 0,5 µm inclus.
PCT/JP2020/001436 2019-02-28 2020-01-17 Nitrure de bore cubique polycristallin et procédé de production associé WO2020174921A1 (fr)

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CN202080010567.0A CN113329985A (zh) 2019-02-28 2020-02-27 立方晶氮化硼多晶体及其制造方法
US17/052,920 US11208324B2 (en) 2019-02-28 2020-02-27 Polycrystalline cubic boron nitride and method for manufacturing the same
EP20762962.7A EP3932893A4 (fr) 2019-02-28 2020-02-27 Nitrure de bore cubique polycristallin et procédé de production associé
PCT/JP2020/008149 WO2020175642A1 (fr) 2019-02-28 2020-02-27 Nitrure de bore cubique polycristallin et procédé de production associé
JP2020541821A JP6798090B1 (ja) 2019-02-28 2020-02-27 立方晶窒化硼素多結晶体及びその製造方法
KR1020217026969A KR102685440B1 (ko) 2019-02-28 2020-02-27 입방정 질화붕소 다결정체 및 그 제조 방법

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