WO2016052497A1 - 焼結体、焼結体を用いた切削工具および焼結体の製造方法 - Google Patents
焼結体、焼結体を用いた切削工具および焼結体の製造方法 Download PDFInfo
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- WO2016052497A1 WO2016052497A1 PCT/JP2015/077494 JP2015077494W WO2016052497A1 WO 2016052497 A1 WO2016052497 A1 WO 2016052497A1 JP 2015077494 W JP2015077494 W JP 2015077494W WO 2016052497 A1 WO2016052497 A1 WO 2016052497A1
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- C04B2235/76—Crystal structural characteristics, e.g. symmetry
- C04B2235/762—Cubic symmetry, e.g. beta-SiC
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/76—Crystal structural characteristics, e.g. symmetry
- C04B2235/767—Hexagonal symmetry, e.g. beta-Si3N4, beta-Sialon, alpha-SiC or hexa-ferrites
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/80—Phases present in the sintered or melt-cast ceramic products other than the main phase
- C04B2235/85—Intergranular or grain boundary phases
Definitions
- the present invention relates to a sintered body, a cutting tool using the sintered body, and a method for manufacturing the sintered body.
- an aluminum oxide (Al 2 O 3 ) sintered body As a material for a cutting tool used for cutting or the like, an aluminum oxide (Al 2 O 3 ) sintered body is known.
- Aluminum oxide sintered bodies are excellent in that they have low reactivity with iron-based work materials and can be manufactured at low cost, but their toughness tends to be low. For this reason, the aluminum oxide sintered body tends to be easily damaged when used as a cutting tool. Furthermore, since the reactivity between aluminum oxide and the metal compound as the binder is low, the nitrides, carbonitrides, etc. of the metals in groups 4A, 5A and 6A of the periodic table are used as the binder. It is difficult to do.
- Patent Document 1 Japanese Patent Laid-Open No. 2013-216517 discloses cubic aluminum nitride, groups 4A and 5A of the periodic table as ceramic sintered bodies having high hardness and toughness. And a ceramic sintered body containing at least one metal compound selected from the group consisting of nitrides, carbides, oxides, borides and solid solutions of Group 6A metals.
- Patent Document 1 uses cubic aluminum nitride having low heat resistance. For this reason, under high-speed cutting conditions when cutting cast cast iron or the like, cubic aluminum nitride in the sintered body is converted to hexagonal aluminum nitride having low hardness. Therefore, there has been a problem that the wear resistance of the sintered body is reduced under high-speed cutting conditions.
- an object of the present invention is to provide a sintered body having excellent wear resistance even under high-speed cutting conditions, a tool using the sintered body, and a method for manufacturing the sintered body.
- the sintered body according to one aspect of the present invention includes a first particle group including particles having a cubic rock salt structure represented by the following formula (1): Al (1-x) Cr x N (1) (In formula (1), x is 0.2 ⁇ x ⁇ 0.8) And a second particle group including particles of at least one first compound selected from the group consisting of oxides or oxynitrides of aluminum, zirconium, yttrium, magnesium, or hafnium.
- a first particle group including particles having a cubic rock salt structure represented by the following formula (1): Al (1-x) Cr x N (1) (In formula (1), x is 0.2 ⁇ x ⁇ 0.8)
- a second particle group including particles of at least one first compound selected from the group consisting of oxides or oxynitrides of aluminum, zirconium, yttrium, magnesium, or hafnium.
- the cutting tool which concerns on 1 aspect of this invention is a cutting tool using the above-mentioned sintered compact.
- a method for manufacturing a sintered body according to one aspect of the present invention is a method for manufacturing the above-described sintered body, and a step of obtaining a first mixed particle group including hexagonal AlN particles and hexagonal Cr 2 N particles.
- a first particle group including particles having a cubic rock salt structure represented by the formula (1); Al (1-x) Cr x N (1) (In formula (1), x is 0.2 ⁇ x ⁇ 0.8)
- a first particle group is mixed with a second particle group containing particles of at least one first compound selected from the group consisting of oxides or oxynitrides of aluminum, zirconium, yttrium, magnesium or hafnium. It is a manufacturing method of a sintered compact provided with the process of obtaining 3 mixed particle groups, and the process of obtaining the sintered compact by sintering the 3rd mixed particle group.
- a method for manufacturing a sintered body according to one aspect of the present invention is a method for manufacturing a sintered body as described above, comprising preparing a target containing aluminum and chromium as constituent elements, and the target including argon. And vapor-phase synthesis of a thin film including a first particle group including particles having a cubic rock salt structure represented by the following formula (1) on a substrate by a physical vapor deposition method in a nitrogen atmosphere: Comprising Al (1-x) Cr x N (1) (In formula (1), x is 0.2 ⁇ x ⁇ 0.8) It is a manufacturing method of a sintered compact.
- a sintered body includes a first particle group including particles having a cubic rock salt structure represented by the following formula (1): Al (1-x) Cr x N (1) (In formula (1), x is 0.2 ⁇ x ⁇ 0.8) And a second particle group including particles of at least one first compound selected from the group consisting of oxides or oxynitrides of aluminum, zirconium, yttrium, magnesium, or hafnium.
- chromium is dissolved in cubic aluminum nitride (hereinafter also referred to as cubic AlN or cAlN) having low heat resistance. And has excellent heat resistance. Therefore, a sintered body using these particles can have excellent wear resistance even under high-speed cutting conditions.
- the x is preferably 0.3 ⁇ x ⁇ 0.7. According to this, the wear resistance of the sintered body is further improved.
- the sintered body has the second particle group of 0.5 volume% or more and 90 volume% or less, and the first compound is Al 2 O 3 , ZrO 2 , AlON, Y 2 O 3 , MgO. And at least one selected from the group consisting of HfO 2 .
- the first compound is Al 2 O 3 , ZrO 2 , AlON, Y 2 O 3 , MgO, HfO 2 .
- the sintered body further includes a third particle group containing cubic boron nitride.
- Cubic boron nitride is a hard particle having better toughness and strength than particles having a cubic rock salt structure represented by the above formula (1). Therefore, when the sintered body contains these particles, the toughness of the sintered body is improved, and thus the fracture resistance is improved.
- the sintered body preferably has the third particle group in an amount of 20% by volume to 70% by volume. According to this, the fracture resistance of the sintered body is further improved.
- a tool according to an aspect of the present invention is a cutting tool using the sintered body according to any one of (1) to (5) above.
- the sintered body is excellent in wear resistance
- a tool using the sintered body is also excellent in wear resistance. Therefore, the tool according to one embodiment of the present invention can have a longer life than the conventional tool.
- a method for manufacturing a sintered body according to one aspect of the present invention is a method for manufacturing a sintered body according to any one of (1) to (5) above, wherein hexagonal AlN particles and hexagonal Cr are used.
- a step of obtaining a first mixed particle group containing 2 N particles, a step of heat-treating the first mixed particle group to obtain a second mixed particle group containing cubic CrN particles, and the second mixed particle group A step of obtaining a first particle group including particles having a cubic rock salt structure represented by the following formula (1) by treatment with a hydrostatic pressure synthesis method or an impact compression method; Al (1-x) Cr x N (1) (In formula (1), x is 0.2 ⁇ x ⁇ 0.8)
- any one of the sintered bodies (1) to (5) can be obtained.
- a method for manufacturing a sintered body according to one aspect of the present invention is a method for manufacturing a sintered body according to any one of (1) to (5) above, wherein the sintered body includes aluminum and chromium as constituent elements.
- the sintered body according to any one of (1) to (5) can be obtained.
- the specific example of the manufacturing method of the sintered compact, tool, and sintered compact concerning embodiment of this invention is demonstrated referring drawings below.
- this invention is not limited to these illustrations, is shown by the claim, and it is intended that all the changes within the meaning and range equivalent to a claim are included.
- the “average particle size” means a value measured by a particle size distribution measuring instrument such as Microtrac.
- the sintered body according to the first embodiment includes a first particle group including particles having a cubic rock salt structure represented by the following formula (1): Al (1-x) Cr x N (1) (In formula (1), x is 0.2 ⁇ x ⁇ 0.8) And a second particle group including particles of at least one first compound selected from the group consisting of oxides or oxynitrides of aluminum, zirconium, yttrium, magnesium, or hafnium.
- Cubic rock salt type crystal structure is a crystal structure typified by rock salt (sodium chloride), and two different face-centered cubic lattices have a length of ridge in the direction of the ridge of the unit cubic lattice. It is a structure that is combined with each other with a half shift.
- the particles (cAlCrN) having a cubic rock salt structure represented by the above formula (1) have a structure in which chromium is dissolved in the crystal structure of cubic aluminum nitride (cAlN). For this reason, the heat resistant temperature of cAlCrN is higher than that of cAlN. Therefore, the sintered body containing cAlCrN can have excellent wear resistance in high-speed cutting.
- x is 0.2 ⁇ x ⁇ 0.8, preferably 0.3 ⁇ x ⁇ 0.7, and more preferably 0.4 ⁇ x ⁇ 0.6.
- x is less than 0.2, the sintered body cannot exhibit excellent wear resistance in high-speed cutting. The reason for this is considered that when x is less than 0.2, the heat resistance of cAlCrN is not sufficiently improved.
- x exceeds 0.8 the sintered body cannot exhibit excellent wear resistance in high-speed cutting. The reason for this is considered to be that when x exceeds 0.8, the hardness of cAlCrN decreases, and the hardness of the sintered body also decreases.
- the sintered body according to the first embodiment preferably contains 20% by volume or more and 99.5% by volume or less, more preferably 35% by volume or more and 99.5% by volume or less of the first particle group. More preferably, it is contained in an amount of not less than volume% and not more than 80 volume%. When the sintered body contains 20% by volume or more of the first particle group, it can have excellent wear resistance in high-speed cutting.
- the sintered body according to the first embodiment includes a second particle group including particles of at least one first compound selected from the group consisting of oxides or oxynitrides of aluminum, zirconium, yttrium, magnesium, or hafnium.
- a second particle group including particles of at least one first compound selected from the group consisting of oxides or oxynitrides of aluminum, zirconium, yttrium, magnesium, or hafnium.
- the 2nd particle group in a sintered compact exists in the interface of adjacent hard particles, and plays the role of a binder phase. Since the binder phase can firmly bond the hard particles, the sintered body can have further excellent wear resistance.
- Examples of the first compound contained in the second particle group include aluminum oxide (Al 2 O 3 ), zirconium oxide (ZrO 2 ), yttrium oxide (Y 2 O 3 ), magnesium oxide (MgO), and hafnium oxide ( HfO 2 ) or the like can be used.
- Al 2 O 3 zirconium oxide
- ZrO 2 zirconium oxide
- Y 2 O 3 yttrium oxide
- MgO magnesium oxide
- hafnium oxide ( HfO 2 ) or the like can be used.
- aluminum oxide (Al 2 O 3 ), yttrium oxide (Y 2 O 3 ), magnesium oxide (MgO), or hafnium oxide (HfO 2 ) is used, the wear resistance of the sintered body is greatly improved.
- the sintered body according to the first embodiment preferably includes the second particle group in an amount of 0.5% to 90% by volume, and more preferably includes 10% to 50% by volume.
- the sintered body contains the second particle group in the range of 0.5 volume% or more and 90 volume% or less, the wear resistance and fracture resistance of the sintered body are further improved.
- the second particle group contains Al 2 O 3 and ZrO 2 , the fracture resistance of the sintered body is greatly improved. A possible reason for this is that Al 2 O 3 is strengthened by dispersion strengthening with ZrO 2 .
- the sintered body according to the first embodiment preferably further has a third particle group containing cubic boron nitride.
- Cubic boron nitride is a hard particle that has better toughness and strength than cAlCrN. Therefore, when the sintered body contains these particles, the toughness of the sintered body is improved, and thus the fracture resistance is improved.
- the third particle group contains cubic boron nitride, the fracture resistance of the sintered body is greatly improved. This may be because the bond between boron and cAlCrN becomes strong.
- the sintered body has 20% by volume or more and 70% by volume or less of the third particle group.
- the sintered body contains 20% by volume or more of the third particle group, the fracture resistance of the sintered body is greatly improved.
- the amount of the third particle group in the sintered body exceeds 70% by volume, the wear resistance is lowered.
- the tool according to the second embodiment is a tool using the sintered body according to the first embodiment.
- the sintered body of the first embodiment is excellent in wear resistance in high-speed cutting, a tool using the sintered body is also excellent in wear resistance.
- Examples of the cutting tool according to the second embodiment may include a drill, an end mill, a milling cutting edge replacement cutting tip, a turning cutting edge replacement cutting tip, a metal saw, a gear cutting tool, a reamer, or a tap. it can. Further, the cutting tool may be entirely constituted by the sintered body, or a part thereof (for example, a blade edge portion) may be constituted by the sintered body.
- the cutting tool can be produced by processing the sintered body into a desired shape.
- the sintered body can be processed by, for example, a laser.
- a cutting tool can be produced by joining a sintered compact to the desired position of the base
- the method for joining the sintered bodies is not particularly limited, but in order to firmly bond the base body and the sintered body between the base body and the sintered body from the viewpoint of suppressing the separation of the sintered body from the base body. It is preferable to interpose a bonding layer.
- the method for producing a sintered body described in the first embodiment is indicated by S1 in FIG. 1 to obtain a first mixed particle group including hexagonal AlN particles and hexagonal Cr 2 N particles.
- the process is also referred to as “a step of obtaining a first mixed particle group”), and a step of heat-treating the first mixed particle group to obtain a second mixed particle group containing cubic CrN particles (in FIG. 1, S2).
- a step of obtaining the second mixed particle group it is also referred to as a “step of obtaining the second mixed particle group”
- the second mixed particle group is treated by a hydrostatic pressure synthesis method or an impact compression method to obtain a cubic represented by the following formula (1).
- a step of obtaining a first particle group containing particles having a crystal rock salt structure shown as S3 in FIG. 1; hereinafter, also referred to as “step of obtaining the first particle group”); Al (1-x) Cr x N (1) (In formula (1), x is 0.2 ⁇ x ⁇ 0.8)
- a step of obtaining a third mixed particle group indicated by S4 in FIG.
- step of obtaining third mixed particles a step of obtaining third mixed particles
- step of obtaining a sintered body a step of obtaining third mixed particles
- Step of obtaining first mixed particle group Referring to FIG. 1, in the step of obtaining the first mixed particle group (S1), hexagonal AlN (hereinafter also referred to as hAlN) particles and hexagonal Cr 2 N (hereinafter also referred to as hCr 2 N) particles are included. A first mixed particle group is obtained.
- the first mixed particle group is preferably mixed using a ball mill device or a bead mill device, and pulverized so that the average particle size is 0.5 ⁇ m or less.
- Step of obtaining second mixed particle group Next, in the step (S2) of obtaining a second mixed particle group, the first mixed particle group is heat-treated to obtain a second mixed particle group containing cubic CrN particles.
- the heat treatment can be performed, for example, by heating the first mixed particle group under a condition of 800 ° C. or higher and 1100 ° C. or lower in a nitrogen atmosphere. As a result, hexagonal Cr 2 N contained in the first mixed particle group is changed to cubic CrN.
- Step of obtaining the first particle group the second mixed particle group is processed by the hydrostatic pressure synthesis method or the impact compression method to obtain the first particle group containing cubic AlCrN particles.
- a second mixed particle group is mixed with a heat sink and copper powder as a pressure medium and filled in a steel container, and instantaneously generated by a shock wave with a pressure of 15 GPa or more and a pressurization time of 50 microseconds or less. Can be carried out by pressurizing to. Thereby, the hexagonal AlN contained in the second mixed particle group is changed to cubic AlN, and Cr is dissolved in the cubic AlN to synthesize cubic AlCrN.
- the pressure of impact pressing is preferably 15 GPa or more and 50 GPa or less, and more preferably 35 GPa or more and 50 GPa or less.
- the temperature at the time of impact pressing is preferably 1200 ° C. or higher and 3000 ° C. or lower, more preferably 1800 ° C. or higher and 2200 ° C. or lower.
- the obtained first particle group is preferably pulverized to an average particle size of 0.1 ⁇ m or more and 0.5 ⁇ m or less by a ball mill device or a bead mill device.
- the first particle group can be used as a raw material for the sintered body.
- Step of obtaining third mixed particle group at least one first particle group selected from the group consisting of the first particle group and an oxide or oxynitride of aluminum, zirconium, yttrium, magnesium, or hafnium.
- a third mixed particle group is obtained by mixing with a second particle group containing particles of one compound.
- the third particle group can further include cubic boron nitride.
- the third mixed particle group is preferably mixed using a ball mill device or a bead mill device and pulverized so that the average particle diameter is 0.5 ⁇ m or less.
- Step of obtaining a sintered body Next, in the step (S5) of obtaining a sintered body, the third mixed particle group is sintered to obtain a sintered body.
- the third mixed particle group can be treated at a pressure of 10 kPa to 15 GPa and a temperature of 800 ° C. to 1900 ° C. to obtain a sintered body.
- the step of obtaining a sintered body is preferably performed in a non-oxidizing atmosphere, and particularly preferably performed in a vacuum or a nitrogen atmosphere.
- the sintering method is not particularly limited, spark plasma sintering (SPS), hot press, ultra-high pressure press, or the like can be used.
- the method for manufacturing a sintered body according to the fourth embodiment includes a step of preparing a target containing aluminum and chromium as constituent elements; A thin film comprising a first group of particles containing particles having a cubic rock salt structure represented by the following formula (1) on a substrate by treating the target by physical vapor deposition in an argon and nitrogen atmosphere. Comprising a step of gas phase synthesis, Al (1-x) Cr x N (1) (In formula (1), x is 0.2 ⁇ x ⁇ 0.8) It is a manufacturing method of a sintered compact.
- the step of vapor-phase synthesizing the thin film containing the first particle group can employ, for example, a method of forming a thin film on a substrate by treating a target with an arc ion plating method.
- the processing conditions at this time may be, for example, Ar flow rate 20 sccm, N 2 flow rate 80 sccm, pressure 2 Pa, bias 110 V, arc current 91 A, and substrate temperature 400 ° C.
- Examples 1 to 42 (Step of obtaining first mixed particle group) Hexagonal AlN particles (KK Tokuyama) and hexagonal Cr 2 N particles (New JIM Co.), 10: 90-90: 10 a first mixed particles were mixed at a ratio of Obtained.
- the first mixed particle group was pulverized by a bead mill so that the average particle size was 0.5 ⁇ m or less.
- Step of obtaining second mixed particle group Next, the first mixed particle group was heat-treated at 900 ° C. in a nitrogen treatment furnace to obtain a second mixed particle group containing cubic CrN particles.
- the ratio of the content (mol%) of hAlN and cCrN in the second mixed particle group of each sample is shown in the “second mixed particle group” column of Table 1.
- Step of obtaining the first particle group Next, the second mixed particle group was mixed with a heat sink and copper powder and filled into a steel container. Thereafter, the second mixed particle group was treated at a pressure of 40 GPa and a temperature of 2000 ° C. by explosion of an explosive to obtain a first particle group.
- the obtained first particle group was analyzed by XRD, cAlCrN was confirmed.
- the 1st particle group was grind
- Step of obtaining third mixed particle group Next, the first particle group, the second particle group, and the third particle group were mixed to obtain a third mixed particle group.
- each compounding quantity and the kind of compound contained in each particle group are as showing in Table 1.
- the third mixed particle group was pulverized by a bead mill so that the average particle size was 0.5 ⁇ m or less.
- Step of obtaining a sintered body Next, the third mixed particle group was filled into a tantalum capsule and sintered using a press machine at a pressure of 7 GPa and a temperature of 1350 ° C. for 15 minutes to obtain a sintered body.
- the obtained sintered body was cut with a laser and finished to prepare a cutting tool having a tool shape CNMA120408 and a negative land of 15 ° ⁇ 0.1 to 0.15 mm.
- a cutting test was performed on centrifugal cast iron under the following cutting conditions, and the flank wear amount ( ⁇ m) after 1.5 km cutting was measured. Moreover, the wear form and the defect
- Step of obtaining third mixed particle group Next, the first particle group, the second particle group, and the third particle group were mixed to obtain a third mixed particle group.
- each compounding quantity and the kind of compound contained in each particle group are as showing in Table 2.
- the third mixed particle group was pulverized by a bead mill so that the average particle size was 0.5 ⁇ m or less.
- Step of obtaining a sintered body Next, the third mixed particle group was filled into a tantalum capsule and sintered using a press machine at a pressure of 7 GPa and a temperature of 1350 ° C. for 15 minutes to obtain a sintered body.
- the obtained sintered body was cut with a laser and finished to prepare a cutting tool having a tool shape CNMA120408 and a negative land of 15 ° ⁇ 0.1 to 0.15 mm.
- a cutting test was performed on centrifugal cast iron under the following cutting conditions, and the flank wear amount ( ⁇ m) after 1.5 km cutting was measured. Moreover, the wear form and the defect
- Step of obtaining the first particle group the target was processed by an arc ion plating method to form a thin film on the high-speed steel substrate.
- the processing conditions were Ar flow rate 20 sccm, N 2 flow rate 80 sccm, pressure 2 Pa, bias 110 V, arc current 91 A, and substrate temperature 400 ° C.
- the thin film formed on the high-speed steel substrate is peeled off from the substrate and collected, and pulverized to a particle size of 0.5 ⁇ m to 3 ⁇ m with a bead mill to form a slurry, and the slurry is dried to thereby form the first particle group Got.
- cAlCrN was confirmed.
- Step of obtaining third mixed particle group Next, the first particle group, the second particle group, and the third particle group were mixed to obtain a third mixed particle group.
- each compounding quantity and the kind of compound contained in each particle group are as showing in Table 3.
- the third mixed particle group was pulverized by a bead mill so that the average particle size was 0.5 ⁇ m or less.
- Step of obtaining a sintered body Next, the third mixed particle group was filled into a tantalum capsule and sintered using a press machine at a pressure of 7 GPa and a temperature of 1350 ° C. for 15 minutes to obtain a sintered body.
- the obtained sintered body was cut with a laser and finished to prepare a cutting tool having a tool shape CNMA120408 and a negative land of 15 ° ⁇ 0.1 to 0.15 mm.
- a cutting test was performed on centrifugal cast iron under the following cutting conditions, and the flank wear amount ( ⁇ m) after 1.5 km cutting was measured. Moreover, the wear form and the defect
- the sintered body containing cubic AlCrN according to an embodiment of the present invention can be widely used for cutting tools.
- it can be used for a drill, an end mill, a cutting edge replacement cutting tip for milling, a cutting edge replacement cutting tip for turning, a metal saw, a gear cutting tool, a reamer, or a tap.
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Abstract
Description
Al(1-x)CrxN・・・(1)
(式(1)中、xは0.2≦x≦0.8である)
アルミニウム、ジルコニウム、イットリウム、マグネシウムまたはハフニウムの酸化物または酸窒化物からなる群より選択される少なくとも1種の第1化合物の粒子を含む第2粒子群とを有する、焼結体である。
本発明の一態様に係る焼結体の製造方法は、上述の焼結体の製造方法であって、六方晶型AlN粒子および六方晶型Cr2N粒子を含む第1混合粒子群を得る工程と、第1混合粒子群を熱処理して、立方晶型CrN粒子を含む第2混合粒子群を得る工程と、第2混合粒子群を静水圧合成法または、衝撃圧縮法で処理して、下記式(1)で表される立方晶岩塩型構造を有する粒子を含む第1粒子群を得る工程と、
Al(1-x)CrxN・・・(1)
(式(1)中、xは0.2≦x≦0.8である)
第1粒子群と、アルミニウム、ジルコニウム、イットリウム、マグネシウムまたはハフニウムの酸化物または酸窒化物からなる群より選択される少なくとも1種の第1化合物の粒子を含む第2粒子群とを混合して第3混合粒子群を得る工程と、第3混合粒子群を焼結して焼結体を得る工程とを備える、焼結体の製造方法である。
Al(1-x)CrxN・・・(1)
(式(1)中、xは0.2≦x≦0.8である)
焼結体の製造方法である。
最初に本発明の実施態様を列記して説明する。
Al(1-x)CrxN・・・(1)
(式(1)中、xは0.2≦x≦0.8である)
アルミニウム、ジルコニウム、イットリウム、マグネシウムまたはハフニウムの酸化物または酸窒化物からなる群より選択される少なくとも1種の第1化合物の粒子を含む第2粒子群とを有する焼結体である。
Al(1-x)CrxN・・・(1)
(式(1)中、xは0.2≦x≦0.8である)
前記第1粒子群と、アルミニウム、ジルコニウム、イットリウム、マグネシウムまたはハフニウムの酸化物または酸窒化物からなる群より選択される少なくとも1種の第1化合物の粒子を含む第2粒子群とを混合して第3混合粒子群を得る工程と、前記第3混合粒子群を焼結して焼結体を得る工程とを備える、焼結体の製造方法である。
Al(1-x)CrxN・・・(1)
(式(1)中、xは0.2≦x≦0.8である)、
焼結体の製造方法である。
[本発明の実施形態の詳細]
本発明の実施形態にかかる焼結体、工具、焼結体の製造方法の具体例を、以下に図面を参照しつつ説明する。なお、本発明はこれらの例示に限定されるものではなく、請求の範囲によって示され、請求の範囲と均等の意味および範囲内でのすべての変更が含まれることが意図される。
第1の実施形態に係る焼結体は、下記式(1)で表される立方晶岩塩型構造を有する粒子を含む第1粒子群と、
Al(1-x)CrxN・・・(1)
(式(1)中、xは0.2≦x≦0.8である)
アルミニウム、ジルコニウム、イットリウム、マグネシウムまたはハフニウムの酸化物または酸窒化物からなる群より選択される少なくとも1種の第1化合物の粒子を含む第2粒子群とを有する焼結体である。
第2の実施形態に係る工具は、第1の実施形態に係る焼結体を用いた工具である。上述のように、第1の実施形態の焼結体は、高速切削における耐摩耗性に優れるため、これを用いた工具もまた、耐摩耗性に優れることとなる。
第3の実施形態に係る焼結体の製造方法について、図1を用いて説明する。
Al(1-x)CrxN・・・(1)
(式(1)中、xは0.2≦x≦0.8である)
前記第1粒子群と、アルミニウム、ジルコニウム、イットリウム、マグネシウムまたはハフニウムの酸化物または酸窒化物からなる群より選択される少なくとも1種の第1化合物の粒子を含む第2粒子群とを混合して第3混合粒子群を得る工程(図1中、S4で示される。以下、「第3混合粒子を得る工程」とも記す)と、前記第3混合粒子群を焼結して焼結体を得る工程(図1中、S5で示される。以下、「焼結体を得る工程」とも記す)とを備える。
図1を参照し、第1混合粒子群を得る工程(S1)において、六方晶型AlN(以下、hAlNとも記す)粒子および六方晶型Cr2N(以下、hCr2Nとも記す)粒子を含む第1混合粒子群を得る。第1混合粒子群は、ボールミル装置やビーズミル装置などを用いて混合し、平均粒子径が0.5μm以下となるように粉砕しておくことが好ましい。
次に、第2混合粒子群を得る工程(S2)において、前記第1混合粒子群を熱処理して、立方晶型CrN粒子を含む第2混合粒子群を得る。
次に、第1粒子群を得る工程(S3)において、第2混合粒子群を静水圧合成法または衝撃圧縮法で処理して、立方晶型AlCrN粒子を含む第1粒子群を得る。
次に、第3混合粒子群を得る工程(S4)において、第1粒子群と、アルミニウム、ジルコニウム、イットリウム、マグネシウムまたはハフニウムの酸化物または酸窒化物からなる群より選択される少なくとも1種の第1化合物の粒子を含む第2粒子群とを混合して第3混合粒子群を得る。
第3混合粒子群は、ボールミル装置やビーズミル装置などを用いて混合し、平均粒子径が0.5μm以下となるように粉砕しておくことが好ましい。
次に、焼結体を得る工程(S5)において、第3混合粒子群を焼結して焼結体を得る。
第4の実施形態に係る焼結体の製造方法は、アルミニウムとクロムを構成元素として含むタ―ゲットを準備する工程と、
前記ターゲッ卜を、アルゴンおよび窒素雰囲気中で、物理蒸着法で処理して、基板上に下記式(1)で表される立方晶岩塩型構造を有する粒子を含む第1粒子群を含む薄膜を気相合成する工程とを備える、
Al(1-x)CrxN・・・(1)
(式(1)中、xは0.2≦x≦0.8である)
焼結体の製造方法である。
(第1混合粒子群を得る工程)
六方晶型AlN粒子((株)トクヤマ製)および六方晶型Cr2N粒子(新日本金属(株)製)を、10:90~90:10の割合で混合して第1混合粒子群を得た。なお、第1混合粒子群はビーズミルにて平均粒径が0.5μm以下になるように粉砕した。
次に、第1混合粒子群を窒素処理炉にて、900℃の条件で熱処理して、立方晶型CrN粒子を含む第2混合粒子群を得た。各試料の第2混合粒子群中のhAlNとcCrNとの含有量(mоl%)の比を、表1の「第2混合粒子群」欄に示す。
次に、第2混合粒子群をヒートシンクおよび銅粉と混合して鋼製容器に充填した。その後、爆薬の爆発により、第2混合粒子群を圧力40GPa、温度2000℃で処理して第1粒子群を得た。得られた第1粒子群をXRD分析したところ、cAlCrNが確認された。なお、第1粒子群はビーズミルにて平均粒径が0.5μm以下になるように粉砕した。
次に、第1粒子群、第2粒子群および第3粒子群を混合して第3混合粒子群を得た。なお、それぞれの配合量、ならびに各粒子群に含まれる化合物の種類は、表1に示すとおりである。なお、第3混合粒子群はビーズミルにて平均粒径が0.5μm以下になるように粉砕した。
次に、第3混合粒子群をタンタル製のカプセルに充填し、プレス機を用いて、圧力7GPaおよび温度1350℃で15分間維持して焼結させ、焼結体を得た。
焼結体をXRD分析し、リートベルト法にて格子定数を精密化し、cAl(1-x)CrxNの格子定数およびxの値を得た。ここで、xの値は、cAlNの格子定数4.12Å、cCrNの格子定数4.15Åに基づき、比例計算によりCrの固溶量を導出して得た。結果を表1に示す。
得られた焼結体を、レーザにて切断して仕上げ加工し、工具形状CNMA120408、ネガランド15°×0.1~0.15mmの切削工具を作製した。得られた切削工具を用いて、以下の切削条件で遠心鋳造鋳鉄の切削試験を行い、1.5km切削後の逃げ面摩耗量(μm)を測定した。また、2.0km切削後の切削工具の摩耗形態および欠損状況を観察した。
切削速度:900m/分
切込み量:0.1mm
送り量:0.28mm/rev
クーラント:エマルジョン
装置:オークマLB400、ホルダー:EWN68-150CKB6
被削材:緻密パーライトの組織を有し、ネズミ鋳鉄の化学組成を有する遠心鋳造鋳鉄
被削材の形状:円筒状、内径φ85mm
結果を表1に示す。
試料1~試料7を比較すると、前記式(1)中のxの値が0.2以上0.8以下であると(試料2~6)、焼結体の耐摩耗性が優れていた。
(第1混合粒子群を得る工程)
六方晶型AlN粒子((株)トクヤマ製)および六方晶型Cr2N粒子(新日本金属(株)製)を、表2の「配合比」に示したAlとCrの原子比となるように混合して第1混合粒子群を得た。なお、第1混合粒子群はビーズミルにて平均粒径が0.5μm以下になるように粉砕した。
(第1粒子群を得る工程)
次に、第1混合粒子群を窒素炉中で、窒素圧力8MPaおよび温度2000℃で処理して第一粒子群を作製した(静圧合成法)。該硬質材料をXRD分析したところ、cAlCrNが確認された。
次に、第1粒子群、第2粒子群および第3粒子群を混合して第3混合粒子群を得た。なお、それぞれの配合量、ならびに各粒子群に含まれる化合物の種類は、表2に示すとおりである。なお、第3混合粒子群はビーズミルにて平均粒径が0.5μm以下になるように粉砕した。
次に、第3混合粒子群をタンタル製のカプセルに充填し、プレス機を用いて、圧力7GPaおよび温度1350℃で15分間維持して焼結させ、焼結体を得た。
焼結体をXRD分析し、リートベルト法にて格子定数を精密化し、cAl(1-x)CrxNの格子定数およびxの値を得た。ここで、xの値は、cAlNの格子定数4.12Å、cCrNの格子定数4.15Åに基づき、比例計算によりCrの固溶量を導出して得た。結果を表2に示す。
得られた焼結体を、レーザにて切断して仕上げ加工し、工具形状CNMA120408、ネガランド15°×0.1~0.15mmの切削工具を作製した。得られた切削工具を用いて、以下の切削条件で遠心鋳造鋳鉄の切削試験を行い、1.5km切削後の逃げ面摩耗量(μm)を測定した。また、2.0km切削後の切削工具の摩耗形態および欠損状況を観察した。
切削速度:900m/分
切込み量:0.1mm
送り量:0.28mm/rev
クーラント:エマルジョン
装置:オークマLB400、ホルダー:EWN68-150CKB6
被削材:緻密パーライトの組織を有し、ネズミ鋳鉄の化学組成を有する遠心鋳造鋳鉄
被削材の形状:円筒状、内径φ85mm
結果を表2に示す。
試料43~試料49を比較すると、前記式(1)中のxの値が0.2以上0.8以下であると(試料44~48)、焼結体の耐摩耗性が優れていた。
(ターゲット準備工程)
ターゲット中のAl、Crの配合比(原子数比)が、表3の「ターゲット組成」欄に記載の割合となるように、ターゲットを準備した。
次に、ターゲットをアークイオンプレーティング法で処理して、高速度鋼基板の上に薄膜を形成した。処理条件は、Ar流量20sccm、N2流量80sccm、圧力2Pa、バイアス110V、アーク電流91A、基板温度400℃であった。次に高速度鋼基板上に形成された薄膜を基板から剥がして回収し、ビーズミルで粒径0.5μm~3μmになるよう粉砕してスラリーを作り、該スラリーを乾燥させることで第1粒子群を得た。これをXRD分析したところ、cAlCrNが確認された。
次に、第1粒子群、第2粒子群および第3粒子群を混合して第3混合粒子群を得た。なお、それぞれの配合量、ならびに各粒子群に含まれる化合物の種類は、表3に示すとおりである。なお、第3混合粒子群はビーズミルにて平均粒径が0.5μm以下になるように粉砕した。
次に、第3混合粒子群をタンタル製のカプセルに充填し、プレス機を用いて、圧力7GPaおよび温度1350℃で15分間維持して焼結させ、焼結体を得た。
焼結体をXRD分析し、リートベルト法にて格子定数を精密化し、cAl(1-x)CrxNの格子定数およびxの値を得た。ここで、xの値は、cAlNの格子定数4.12Å、cCrNの格子定数4.15Åに基づき、比例計算によりCrの固溶量を導出して得た。結果を表3に示す。
得られた焼結体を、レーザにて切断して仕上げ加工し、工具形状CNMA120408、ネガランド15°×0.1~0.15mmの切削工具を作製した。得られた切削工具を用いて、以下の切削条件で遠心鋳造鋳鉄の切削試験を行い、1.5km切削後の逃げ面摩耗量(μm)を測定した。また、2.0km切削後の切削工具の摩耗形態および欠損状況を観察した。
切削速度:900m/分
切込み量:0.1mm
送り量:0.28mm/rev
クーラント:エマルジョン
装置:オークマLB400、ホルダー:EWN68-150CKB6
被削材:緻密パーライトの組織を有し、ネズミ鋳鉄の化学組成を有する遠心鋳造鋳鉄
被削材の形状:円筒状、内径φ85mm
結果を表3に示す。
試料85~試料91を比較すると、前記式(1)中のxの値が0.2以上0.8以下であると(試料2~6)、焼結体の耐摩耗性が優れていた。
Claims (8)
- 下記式(1)で表される立方晶岩塩型構造を有する粒子を含む第1粒子群と、
Al(1-x)CrxN・・・(1)
(式(1)中、xは0.2≦x≦0.8である)
アルミニウム、ジルコニウム、イットリウム、マグネシウムまたはハフニウムの酸化物または酸窒化物からなる群より選択される少なくとも1種の第1化合物の粒子を含む第2粒子群とを有する、
焼結体。 - 前記xは、0.3≦x≦0.7である、請求項1に記載の焼結体。
- 前記焼結体は、前記第2粒子群を0.5体積%以上90体積%以下有し、
前記第1化合物は、Al2O3、ZrO2、AlON、Y2O3、MgOおよびHfO2からなる群より選択される少なくとも1種を含む、請求項1または請求項2に記載の焼結体。 - 前記焼結体は、さらに立方晶型窒化ホウ素を含む第3粒子群を有する、請求項1~請求項3のいずれか1項に記載の焼結体。
- 前記焼結体は、前記第3粒子群を20体積%以上70体積%以下有する、請求項4に記載の焼結体。
- 請求項1~請求項5のいずれか1項に記載の焼結体を用いた切削工具。
- 請求項1~請求項5のいずれか1項に記載の焼結体の製造方法であって、
六方晶型AlN粒子および六方晶型Cr2N粒子を含む第1混合粒子群を得る工程と、
前記第1混合粒子群を熱処理して、立方晶型CrN粒子を含む第2混合粒子群を得る工程と、
前記第2混合粒子群を静水圧合成法または衝撃圧縮法で処理して、下記式(1)で表される立方晶岩塩型構造を有する粒子を含む第1粒子群を得る工程と、
Al(1-x)CrxN・・・(1)
(式(1)中、xは0.2≦x≦0.8である)
前記第1粒子群と、アルミニウム、ジルコニウム、イットリウム、マグネシウムまたはハフニウムの酸化物または酸窒化物からなる群より選択される少なくとも1種の第1化合物の粒子を含む第2粒子群とを混合して第3混合粒子群を得る工程と、
前記第3混合粒子群を焼結して焼結体を得る工程とを備える、
焼結体の製造方法。 - 請求項1~請求項5のいずれか1項に記載の焼結体の製造方法であって、
アルミニウムとクロムを構成元素として含むタ―ゲットを準備する工程と、
前記ターゲッ卜を、アルゴンおよび窒素雰囲気中で、物理蒸着法で処理して、基板上に下記式(1)で表される立方晶岩塩型構造を有する粒子を含む第1粒子群を含む薄膜を気相合成する工程とを備える、
Al(1-x)CrxN・・・(1)
(式(1)中、xは0.2≦x≦0.8である)
焼結体の製造方法。
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KR20170063819A (ko) | 2017-06-08 |
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