JP6064482B2 - Ceramic sintered body, method for producing the same, and tool - Google Patents

Description

  The present invention relates to a ceramic sintered body, a method for manufacturing the same, and a tool, and more particularly, to a ceramic sintered body containing aluminum oxynitride, a method for manufacturing the same, and a tool.

  The atmospheric pressure phase aluminum oxynitride has a low coefficient of thermal expansion and low reactivity with iron. Due to its characteristics, use of aluminum oxynitride in the atmospheric pressure phase as a cutting tool material has been studied, but the hardness of the cutting tool material is inadequate with a Vickers hardness of about 1900 Hv. It is said that the desired hardness of the cutting tool is about 4 times that of the workpiece. A hardened steel, which is an example of a workpiece, has a Rockwell hardness of 50 HRC or more and a Vickers hardness conversion of 600 Hv or more. Therefore, the cutting tool needs to possess a hardness of 2400 Hv or more. Accordingly, the normal pressure phase aluminum oxynitride cannot be used for a high-hardness workpiece due to lack of plastic deformation resistance due to insufficient hardness. For example, Tadaaki Sugita and two others, “Basic Cutting Processing Science”, Kyoritsu Shuppan, p115, describe that a hardness about 4 times that of the workpiece is required. Further, regarding hardness and thermal expansion coefficient of aluminum oxynitride in the atmospheric pressure phase, for example, Corvin (Normand D. Corbin), “Aluminum Oxynitride Spinel A Review”, Journal of European Ceramic Society (Journal of Europe). (Ceramic Society), UK, 1989, 5, p. 143-154.

  Japanese Unexamined Patent Application Publication No. 2007-533593 also discloses a ceramic body made of aluminum oxynitride reinforced by including silicon carbide whiskers. However, this improves the fracture toughness and can only be expected to suppress the progress immediately after the occurrence of defects and cracks. Moreover, since it contains silicon carbide having high reactivity with iron, it contains iron such as chromium steel (SCr), chromium molybdenum steel (SCM), nickel chromium steel (SNC), stainless steel (SUS), etc. It is not suitable for cutting tools made of ferrous materials.

JP 2007-533593 A

Corbin, "Aluminum Oxynitride Spinel: A Review", Journal of European Ceramic Society, Journal of European Ceramic Society, 5 years, 1988, UK. 143-154 Tadaaki Sugita, two others, "Basic Cutting Processing", Kyoritsu Publishing, p115

  The present invention has been made to solve the above-described problems. A main object of the present invention is to provide a high-hardness ceramic sintered body having low reactivity with iron, a method for producing the same, and a tool.

  The ceramic sintered body according to the present invention contains aluminum oxynitride and has a Vickers hardness of 2400 Hv or more. In this way, a ceramic sintered body having high hardness and low reactivity with iron can be obtained, which is optimal for a cutting tool made of iron-based material.

  The ceramic sintered body is a transition element of Group 4, Group 5, Group 6, or aluminum, silicon, boron, or nitrides, carbides, carbonitrides, borides, oxides, oxynitrides thereof. Or at least one of a compound, an intermetallic compound, or a composite compound thereof. Thereby, it can be baked firmly, maintaining the high hardness which high pressure phase aluminum oxynitride has with the material mentioned above.

  Furthermore, the ceramic sintered body may include at least one of aluminum nitride and aluminum oxide. Thus, even if any one of aluminum nitride and aluminum oxide, which are starting materials for constituting aluminum oxynitride, remains in the ceramic sintered body to some extent, the effect of the present invention can be obtained.

  The composition ratio of oxygen atoms to nitrogen atoms contained in the aluminum oxynitride can be 3 or more and 9 or less.

  The tool which concerns on this invention consists of the said ceramic sintered compact. In this way, a tool capable of cutting a ferrous material with high hardness can be realized.

  The method for producing a ceramic sintered body according to the present invention comprises a step of preparing a precursor and producing a normal pressure phase aluminum oxynitride powder or a first composite powder containing normal pressure phase aluminum oxynitride, and a normal pressure phase acid. A step of producing a high-pressure-phase aluminum oxynitride powder or a high-pressure-phase aluminum oxynitride-containing composite powder from the first composite powder containing aluminum nitride powder or atmospheric pressure-phase aluminum oxynitride; A step of sintering a composite powder containing aluminum oxynitride to produce a sintered body. If it does in this way, the ceramic sintered compact according to this invention can be obtained easily.

  The step of producing the normal pressure phase aluminum oxynitride powder or the first composite powder containing the normal pressure phase aluminum oxynitride has a composition ratio of oxygen atoms to nitrogen atoms contained in the high pressure phase aluminum oxynitride of 3 to 9 A step of preparing the precursor may be included. In addition, the step of producing the normal pressure phase aluminum oxynitride powder or the first composite powder containing the normal pressure phase aluminum oxynitride is usually performed by firing the precursor under the condition of a heating temperature of 1600 ° C. or more and 2000 ° C. or less. A step of producing a first composite powder containing the pressure phase aluminum oxynitride powder or the atmospheric pressure phase aluminum oxynitride may be included. Thereby, the atmospheric pressure phase aluminum oxynitride powder or the first composite powder containing the atmospheric pressure phase aluminum oxynitride having an appropriate composition ratio of oxygen atoms and nitrogen atoms can be produced. In addition, the step of preparing the atmospheric pressure phase aluminum oxynitride powder or the first composite powder containing the atmospheric pressure phase aluminum oxynitride includes the precursor, the atmospheric pressure phase aluminum oxynitride powder, or the first composite powder. At least one of Group 4, Group 5, Group 6 transition metal, or aluminum, silicon, boron, or a nitride, carbide, carbonitride, boride, oxide, acid thereof A step of adding at least one of a nitride, an intermetallic compound, or a composite compound thereof may be included.

  The step of producing the high-pressure phase aluminum oxynitride powder or the composite powder containing the high-pressure phase aluminum oxynitride includes the normal pressure phase aluminum oxynitride powder instantaneously by a shock wave having a pressure of 15 GPa or more and a pressurization time of 50 μsec or less, or Pressurizing the first composite powder containing normal pressure phase aluminum oxynitride and using the ultrahigh pressure generator, the normal pressure phase aluminum oxynitride powder at a pressure of 10 GPa or more and a temperature of 1200 ° C. or more and 2000 ° C. or less; From the step of pressurizing the first composite powder containing the pressure phase aluminum oxynitride and the step of causing the carrier gas flow rate to 1 SLM and colliding with the substrate at a particle velocity of 150 m / s or more using the aerosol deposition method. One selected from the group may be included. Thereby, a high-pressure phase aluminum oxynitride powder or a composite powder containing high-pressure phase aluminum oxynitride can be produced.

  The step of producing the high-pressure phase aluminum oxynitride powder or the second composite powder containing high-pressure phase aluminum oxynitride includes the high-pressure phase aluminum oxynitride powder or the second composite powder containing high-pressure phase aluminum oxynitride. In addition, transition metals of Group 4, Group 5, Group 6, or aluminum, silicon, boron, or nitrides, carbides, carbonitrides, borides, oxides, oxynitrides, and intermetallic compounds thereof Or a step of adding at least one of the complex compounds.

  The step of producing the sintered body is performed at a pressure of 1 GPa or higher and a temperature of 1100 ° C. or higher and 2000 ° C. or lower using an ultrahigh pressure generator, or a pressure of 10 MPa or higher and a temperature of 800 ° C. or higher and 1800 ° C. or lower using a discharge plasma sintering apparatus The step of sintering the high-pressure phase aluminum oxynitride powder or the second composite powder containing the high-pressure phase aluminum oxynitride may be included.

  A method for producing a ceramic sintered body according to another aspect of the present invention includes a step of preparing a precursor from a starting material containing at least one of aluminum nitride and aluminum oxide, and the phase of the precursor into a high-pressure phase. And a step of sintering at the same time as the transition to produce a sintered body. Thereby, the ceramic sintered compact according to this invention can be obtained easily.

Process for producing the sintered body, the pressure 10GPa or more using a high-pressure apparatus, temperature 1 2 00 ° C. or higher 2000 ° C. or less, the processing time of 20 minutes or more, at the same time the precursor phase transition into the high-pressure phase the You may include the process of producing a sintered compact.

  Since the ceramic sintered body of the present invention has the high-pressure phase aluminum oxynitride, it has no reactivity with the iron-based material and can have high hardness. Moreover, the tool of this invention can implement | achieve the tool which can cut an iron-type material with high hardness by using the ceramic sintered compact of this invention.

  Since the method for producing a ceramic sintered body according to the present invention includes a step of producing high-pressure phase aluminum oxynitride, a high-hardness ceramic sintered body having no reactivity with iron-based materials can be produced.

It is a flowchart which shows the manufacturing method of the ceramic sintered compact which concerns on this Embodiment. It is a flowchart which shows the manufacturing method of the ceramic sintered compact which concerns on this Embodiment. It is a flowchart which shows the modification of the manufacturing method of the ceramic sintered compact concerning this Embodiment.

  Hereinafter, embodiments of the present invention will be described with reference to the drawings. In the following drawings, the same or corresponding parts are denoted by the same reference numerals, and description thereof will not be repeated.

  First, the ceramic sintered body according to the embodiment will be described. The ceramic sintered body according to the present embodiment can be used as a material for a cutting tool (particularly a tool for cutting an iron-based material), and includes high-pressure phase aluminum oxynitride. The high pressure phase aluminum oxynitride is superior in plastic deformation resistance because of its high hardness compared to the normal pressure phase aluminum oxynitride, and the low pressure phase aluminum oxynitride has low reactivity with iron. Also has characteristics. Therefore, the ceramic sintered body containing the high-pressure phase aluminum oxynitride can be used for a cutting tool with high hardness capable of cutting an iron-based material.

  The ceramic sintered body is a transition element of Group 4, Group 5, Group 6, or aluminum, silicon, boron, or nitrides, carbides, carbonitrides, borides, oxides, oxynitrides thereof. Or at least one of a compound, an intermetallic compound, or a composite compound thereof. Group 4, Group 5 and Group 6 transition elements include, for example, Group 4 transition metal, titanium (Ti), zirconium (Zr), hafnium (Hf), Group 5 transition metal, Vanadium (V), niobium (Nb), tantalum (Ta), and at least one metal selected from chromium (Cr), molybdenum (Mo), and tungsten (W) as a Group 6 transition metal.

Examples of the nitride include titanium nitride (TiN), zirconium nitride (ZrN), hafnium nitride (HfN), vanadium nitride (VN), niobium nitride (NbN), tantalum nitride (TaN), and chromium nitride (Cr). ₂ N), molybdenum nitride (MoN), tungsten nitride (WN), aluminum nitride (AlN), silicon nitride (Si ₃ N ₄ ), and boron nitride (BN). Examples of the carbide include titanium carbide (TiC), zirconium carbide (ZrC), hafnium carbide (HfC), vanadium carbide (VC), niobium carbide (NbC), tantalum carbide (TaC), and chromium carbide (Cr ₃ ). C ₂ ), molybdenum carbide (Mo ₂ C), and tungsten carbide (WC). Examples of the boride include titanium boride (TiB ₂ ), zirconium boride (ZrB ₂ ), hafnium boride (HfB ₂ ), vanadium boride (VB), niobium boride (NbB ₂ ), and boron. Mention may be made of tantalum boride (TaB ₂ ), chromium boride (CrB ₂ ), molybdenum boride (MoB) and tungsten boride (WB). In addition, these metal oxides are titanium oxide (TiO ₂ ), zirconium oxide (ZrO ₂ ), hafnium oxide (HfO ₂ ), vanadium oxide (V ₂ O ₅ ), niobium oxide (Nb ₂ O ₅ ), Tantalum oxide (Ta ₂ O ₅ ), chromium oxide (Cr ₂ O ₃ ), molybdenum oxide (MoO ₃ ), tungsten oxide (WO ₃ ), and the like are used. The composite compounds of these metals include titanium zirconium nitride (TiZrN), titanium hafnium nitride (TiHfN), titanium vanadium nitride (TiVN), titanium niobium nitride (TiNbN), titanium tantalum nitride (TiTaN), titanium nitride chromium (TiCrN). ), Titanium molybdenum nitride (TiMoN), titanium tungsten nitride (TiWN), zirconium hafnium nitride (ZrHfN), zirconium vanadium nitride (ZrVN), zirconium niobium nitride (ZrNbN), zirconium tantalum nitride (ZrTaN), zirconium nitride chromium (ZrCrN) , Zirconium molybdenum nitride (ZrMoN), zirconium tungsten nitride (ZrWN), hafnium vanadium nitride (HfVN), hafnium niobium nitride (HfNbN) , Hafnium tantalum nitride (HfTaN), hafnium chromium nitride (HfCrN), hafnium molybdenum nitride (HfMoN), hafnium tungsten nitride (HfWN), vanadium niobium nitride (VNbN), vanadium tantalum nitride (VTaN), vanadium chromium nitride (VCrN), Vanadium molybdenum nitride (VMoN), vanadium tungsten nitride (VWN), niobium tantalum nitride (NbTaN), niobium chromium nitride (NbCrN), niobium molybdenum nitride (NbMoN), niobium tungsten nitride (NbWN), tantalum chromium nitride (TaCrN), tantalum nitride Molybdenum (TaMoN), tantalum tungsten nitride (TaWN), chromium nitride molybdenum (CrMoN), chromium tungsten nitride (CrWN), molybdenum nitride It refers to such Denkuromu (MoWN). Examples of the oxynitride include titanium oxynitride (TiON), zirconium oxynitride (ZrON), hafnium oxynitride (HfON), vanadium oxynitride (VON), niobium oxynitride (NbON), tantalum oxynitride (TaON), Examples thereof include chromium oxynitride (CrON), molybdenum oxynitride (MoON), tungsten oxynitride (WON), silicon oxynitride (SiON), and boron oxynitride (BON).

  The ceramic sintered body has, as an additive, a transition element of Group 4, Group 5, Group 6, or aluminum, silicon, boron, or a nitride, carbide, carbonitride, boride thereof, By including at least one of the intermetallic compounds, it is possible to increase the strength of the ceramic sintered body while maintaining the high hardness of the high-pressure phase aluminum oxynitride. Therefore, since the tool using this ceramic sintered body is excellent in plastic deformation resistance, the life can be extended.

  Furthermore, the ceramic sintered body may include at least one of aluminum nitride and aluminum oxide. Preferably, the total content of aluminum nitride and aluminum oxide in the ceramic sintered body is 10% or less. At this time, the composition ratio in the ceramic sintered body can be, for example, 60% or more for the aluminum oxynitride and about 30% for the additive. When the proportion of aluminum oxynitride is lower than 50%, the effect of the high-pressure phase aluminum oxynitride is reduced, and the hardness of the ceramic sintered body is lowered.

  The composition ratio of oxygen atoms to nitrogen atoms contained in the high-pressure phase aluminum oxynitride is preferably 3 or more and 9 or less. If the ratio of nitrogen or oxygen is higher than the composition ratio range, the spinel structure of the aluminum oxynitride in the high pressure phase cannot be maintained, the hardness is lowered, and the characteristics of aluminum oxide inferior in fracture resistance are approached.

  As described above, the ceramic sintered body according to the present embodiment can have high hardness by including aluminum oxynitride in a high-pressure phase. Furthermore, the ceramic sintered body can be surely made to have high hardness while suppressing the reactivity with iron by including the above-mentioned additive other than silicon carbide. As a result, the ceramic sintered body according to the present embodiment can be applied to a cutting tool, for example.

  Next, with reference to FIGS. 1-3, the manufacturing method of the ceramic sintered compact concerning this Embodiment is demonstrated.

  As shown in FIG. 1, the method for manufacturing a ceramic sintered body according to the present embodiment prepares a precursor, and uses an atmospheric pressure phase aluminum oxynitride powder or an atmospheric pressure phase aluminum oxynitride powder as a first composite powder. A high-pressure phase aluminum oxynitride powder or a high-pressure phase aluminum oxynitride-containing composite powder is prepared from the manufacturing step (S10) and the first-phase composite powder containing normal-pressure phase aluminum oxynitride powder or normal-pressure phase aluminum oxynitride Step (S20) and step (S30) of producing a sintered body from a high-pressure phase aluminum oxynitride powder or a composite powder containing high-pressure phase aluminum oxynitride, or a high-pressure phase aluminum oxynitride from a precursor as described later And a step of simultaneously performing the production of the sintered body.

  In the step (S10) of preparing the precursor and producing a normal pressure phase aluminum oxynitride powder or a composite powder containing normal pressure phase aluminum oxynitride, the composition ratio of oxygen atoms to nitrogen atoms contained in the high pressure phase aluminum oxynitride A step of producing a precursor (S11) may be included so that becomes 3 or more and 9 or less. At this time, the step (S11) can employ a step of mixing the aluminum nitride powder and the aluminum oxide powder, or a step of increasing the amount of adsorbed oxygen in the aluminum nitride powder. Specific examples of the step of increasing the amount of adsorbed oxygen in the aluminum nitride powder include a method of heat-treating the powder in the air, and a method of exposing the aluminum nitride powder for a certain period of time in a humidity-controlled place. When the process is performed, the amount of adsorbed oxygen can be increased in a short time by pulverizing the powder to increase the surface area of the powder.

  Referring to FIG. 2, at this time, the step of preparing the above precursor and producing a normal pressure phase aluminum oxynitride powder or a composite powder containing normal pressure phase aluminum oxynitride (S10) is included in aluminum oxynitride. A step (S11) of preparing a precursor by mixing aluminum nitride powder and aluminum oxide powder so that the composition ratio of oxygen atoms to nitrogen atoms is 3 or more and 9 or less may be included. Step (S11) is a method of mixing aluminum nitride powder and aluminum oxide powder as described above as long as the composition ratio of oxygen atoms to nitrogen atoms contained in aluminum oxynitride can be 3 or more and 9 or less. Not limited to. The step of producing the precursor (S11) may be a step of producing the precursor by increasing the amount of adsorbed oxygen in the aluminum nitride powder.

  After the precursor is produced as described above, the precursor is fired at a heating temperature of 1600 ° C. or more and 2000 ° C. or less, so that the atmospheric pressure phase aluminum oxynitride powder or the atmospheric pressure phase aluminum oxynitride is added. The step (S13) of producing one composite powder may be included. In steps (S11) and (S12) in FIG. 2, a spinel type aluminum oxynitride can be manufactured by adjusting the composition ratio of oxygen atoms to nitrogen atoms contained in the aluminum oxynitride to be within the above range. Outside the above range, spinel-type aluminum oxynitride is not produced, and in this case, the ceramic sintered body may not have sufficient hardness as a cutting tool material.

  Furthermore, the step of preparing the precursor and producing the atmospheric pressure phase aluminum oxynitride powder or the first composite powder containing the atmospheric pressure phase aluminum oxynitride (S10) is a step of adding a transition metal or the like (S12) (S14). ) May be included. Specifically, as shown in FIG. 2, after the step of preparing the precursor (S11), before the step of firing the precursor (S13), after the step of firing the precursor (S13). Before the step (S20) of producing the high-pressure phase aluminum oxynitride powder or the second composite powder containing the high-pressure phase aluminum oxynitride, the transition elements of Group 4, Group 5, and Group 6 are used as additives. Or adding at least one of aluminum, silicon, boron, or a nitride, carbide, carbonitride, boride, oxide, oxynitride, intermetallic compound, or composite compound thereof Also good. That is, the additive may be added to at least one of the precursor, the atmospheric pressure phase aluminum oxynitride powder, and the first composite powder. These step (S12) and step (S14) may be performed subsequent to the above step (S11) and step (S13), respectively. In the step (S11), the additive may be mixed with aluminum nitride and aluminum oxide powder to produce a precursor, or after the additive is added to the aluminum nitride powder, the amount of adsorbed oxygen is increased. The precursor may be produced by Thereby, since the atmospheric pressure phase aluminum oxynitride obtained by the said process (S13) contains the said additive, the ceramic sintered compact obtained in the process (S30) shown in FIG. 1 is the high pressure containing the said additive. It will contain phase aluminum oxynitride. As a result, the bonding strength between the atmospheric pressure phase aluminum oxynitride and the additive is increased, and the strength can be increased by maintaining the hardness while maintaining the hardness. The material is high and has excellent plastic deformation resistance.

  Next, the high-pressure phase aluminum oxynitride powder or the second composite powder containing high-pressure phase aluminum oxynitride from the normal-pressure phase aluminum oxynitride powder or the first composite powder containing normal-pressure phase aluminum oxynitride shown in FIG. The manufacturing step (S20) will be described. In this step, the atmospheric pressure phase aluminum oxynitride contained in the powder produced in the step (S10) is phase-transduced to produce a high pressure phase aluminum oxynitride.

  A high-pressure phase aluminum oxynitride powder or a high-pressure phase aluminum oxynitride powder or a second composite powder containing a high-pressure phase aluminum oxynitride is prepared from the normal pressure phase aluminum oxynitride powder or the first composite powder containing normal pressure phase aluminum oxynitride shown in FIG. The step (S20) of performing can include a step using an ultrahigh pressure generator or an aerosol deposition method.

  Examples of the ultra-high pressure generator include a method of pressurizing with a shock wave, a multi-anvil device, a belt device, and a piston cylinder device.

  As a specific example, a step of instantaneously pressurizing the normal pressure phase aluminum oxynitride powder or the first composite powder containing the normal pressure phase aluminum oxynitride with a shock wave having a pressure of 10 GPa or more and a pressurization time of 50 μsec or less, Using an anvil device, pressurizing under the conditions of pressure of 10 GPa or more, temperature of 1200 ° C. or more and 2000 ° C. or less, and processing time of 20 minutes or more, flow rate of carrier gas using aerosol deposition method is 1 SLM or more, particle velocity For example, a step of causing collision at 150 m / s or more.

  Furthermore, the process of producing the high pressure phase aluminum oxynitride powder or the 2nd composite powder containing high pressure phase aluminum oxynitride from the 1st composite powder containing a normal pressure phase aluminum oxynitride powder or a normal pressure phase aluminum oxynitride (S20) ) May include a step (S22) of adding a transition metal or the like. Specifically, as shown in FIG. 2, the high-pressure phase aluminum oxynitride powder or the second composite powder containing the high-pressure phase aluminum oxynitride, which is carried out following the step (S21), is used as an additive. Group 4, Group 5, Group 6 transition element, or aluminum, silicon, boron, or nitrides, carbides, carbonitrides, borides, oxides, oxynitrides, intermetallic compounds, or A step of adding a transition metal or the like (S22) for further mixing at least one of the composite compounds may be included. Thereby, since the high-pressure phase aluminum oxynitride obtained by the step (S21) contains the additive, the ceramic sintered body obtained in the step (S30) shown in FIG. 1 has a high-pressure phase containing the additive. It contains aluminum oxynitride. As a result, the bonding strength between the high-pressure phase aluminum oxynitride and the additive is increased, and the ceramic sintered body has high strength and excellent plastic deformation resistance because it can be baked more firmly while maintaining the hardness. Become a material.

  Next, a step (S30) of preparing a sintered body by preparing a high-pressure phase aluminum oxynitride powder or a second composite powder containing high-pressure phase aluminum oxynitride will be described with reference to FIG. In this step, the high-pressure phase aluminum oxynitride powder or the second composite powder containing the high-pressure phase aluminum oxynitride is sintered to produce a sintered body containing the high-pressure phase aluminum oxynitride.

  The step (S30) of preparing the sintered body by preparing the high-pressure phase aluminum oxynitride powder or the second composite powder containing the high-pressure phase aluminum oxynitride shown in FIG. A step (S31) of sintering the molded body at a pressure of 1 GPa or higher and a temperature of 1100 ° C. or higher and 2000 ° C. or lower using a sintering apparatus, or at a pressure of 10 MPa or higher and a temperature of 800 ° C. or higher and 1800 ° C. or lower using a discharge plasma sintering apparatus. May be included.

  At this time, in the step (S21), when the high-pressure phase aluminum oxynitride is obtained as a bulk body, the bulk body is pulverized into a powder form and then mixed with the additive. Sintering the high pressure phase aluminum oxynitride powder mixed with the high pressure phase aluminum oxynitride and the additive or the second composite powder containing the high pressure phase aluminum oxynitride by the step (S22) in the step (S31). Thus, a ceramic sintered body containing high-pressure aluminum oxynitride containing the additive can be obtained.

  Next, another example of the method for manufacturing a ceramic sintered body according to the present embodiment will be described with reference to FIG. In another example of the method for producing a ceramic sintered body according to the present embodiment, a precursor is prepared, and the phase transition from the precursor to the high-pressure phase and the production of the sintered body are performed at the same time. A sintered body having aluminum is produced.

  The step (S11) for producing the precursor of FIG. 3 and the step (S12) for adding a transition metal and the like are the same as the steps included in the step (S10) described in FIG. 1 and FIG. In the process of simultaneously converting and sintering the high-pressure phase into aluminum oxynitride, the precursor was subjected to a pressure of 10 GPa or more, a temperature of 1200 ° C. to 2000 ° C., and a treatment time of 20 minutes or more using an ultrahigh pressure generator. This is a step of pressurizing under conditions (S32), and thus the ceramic sintered body according to the present invention can be produced.

  That is, the method for producing a ceramic sintered body according to the present embodiment can produce a ceramic sintered body having excellent characteristics as compared with conventional aluminum oxynitride and sufficient characteristics as a cutting tool. it can.

  Here, although there is a part which overlaps with embodiment mentioned above, the characteristic structure of this invention is enumerated.

  The ceramic sintered body according to the present invention contains aluminum oxynitride and has a Vickers hardness of 2400 Hv or more. In this way, a ceramic sintered body having high hardness and low reactivity with iron can be obtained, which is optimal for a cutting tool made of iron-based material.

  The ceramic sintered body is a transition element of Group 4, Group 5, Group 6, or aluminum, silicon, boron, or nitrides, carbides, carbonitrides, borides, oxides, oxynitrides thereof. Or at least one of a compound, an intermetallic compound, or a composite compound thereof. Thereby, it can be baked firmly, maintaining the high hardness which high pressure phase aluminum oxynitride has with the material mentioned above.

  The ceramic sintered body may further include at least one of aluminum nitride and aluminum oxide. Thus, even if any one of aluminum nitride and aluminum oxide, which are starting materials for constituting aluminum oxynitride, remains in the ceramic sintered body to some extent, the effect of the present invention can be obtained.

  The composition ratio of oxygen atoms to nitrogen atoms contained in the aluminum oxynitride can be 3 or more and 9 or less. Thereby, the hardness of a ceramic sintered compact can be adjusted by adjusting the said composition ratio.

  The tool which concerns on this invention consists of the said ceramic sintered compact. In this way, a tool capable of cutting a ferrous material with high hardness can be realized.

  The method for producing a ceramic sintered body according to the present invention comprises preparing a precursor from a starting material containing at least one of aluminum nitride and aluminum oxide, and using the precursor to normal pressure phase aluminum oxynitride powder, or normal pressure From the step (S10) of producing a first composite powder containing phase aluminum oxynitride, and from the first composite powder containing atmospheric pressure phase aluminum oxynitride powder or atmospheric pressure phase aluminum oxynitride, high pressure phase aluminum oxynitride A step of producing a second composite powder containing powder or high-pressure phase aluminum oxynitride (S20), and sintering the second composite powder containing high-pressure phase aluminum oxynitride powder or high-pressure phase aluminum oxynitride And a step (S30) of producing a sintered body. If it does in this way, the ceramic sintered compact according to this invention can be obtained easily.

  In the step (S10) of producing the normal pressure phase aluminum oxynitride powder or the first composite powder containing the normal pressure phase aluminum oxynitride, the composition ratio of oxygen atoms to nitrogen atoms contained in the high pressure phase aluminum oxynitride is 3 or more. A step (S11) of producing a precursor so as to be 9 or less may be included. In addition, the precursor is fired at a heating temperature of 1600 ° C. or more and 2000 ° C. or less, thereby producing a normal pressure phase aluminum oxynitride powder or a first composite powder containing normal pressure phase aluminum oxynitride (S13). And may be included. By doing in this way, the ceramic sintered compact containing spinel type aluminum oxynitride can be produced, and this ceramic sintered compact can have sufficient hardness as a material for cutting tools.

  The step (S10) for producing the above-mentioned atmospheric pressure phase aluminum oxynitride powder or the first composite powder containing atmospheric pressure phase aluminum oxynitride is carried out by converting the aluminum nitride and the aluminum oxide into those of Groups 4, 5, and 6. Add at least one of transition metal, aluminum, silicon, boron, or nitrides, carbides, carbonitrides, borides, oxides, oxynitrides, intermetallic compounds, or composite compounds thereof Step (S12) to include may be included. As a result, the bonding strength between the atmospheric pressure phase aluminum oxynitride and the additive is increased, and the strength can be increased by maintaining the hardness while maintaining the hardness. The material is high and has excellent plastic deformation resistance.

  In the step (S20) of producing the high-pressure phase aluminum oxynitride powder or the second composite powder containing the high-pressure phase aluminum oxynitride, the normal pressure is instantaneously generated by a shock wave having a pressure of 10 GPa or more and a pressurization time of 50 μsec or less. Pressurizing the first composite powder containing phase aluminum oxynitride powder or atmospheric pressure phase aluminum oxynitride, and using the ultrahigh pressure generator, the pressure is 10 GPa or more, and the temperature is 1200 ° C. or more and 2000 ° C. or less. Using the step of pressurizing the first composite powder containing aluminum oxynitride powder or atmospheric pressure phase aluminum oxynitride and the aerosol deposition method, the flow rate of the carrier gas is 1 SLM, and the particle velocity is 150 m / s or more. One selected from the group consisting of the step of causing the substrate to collide with the substrate may be included.

  The step (S20) of producing the high-pressure phase aluminum oxynitride powder or the second composite powder containing the high-pressure phase aluminum oxynitride includes a transition metal of Group 4, Group 5, Group 6, aluminum, silicon And adding at least one of boron, or nitrides, carbides, carbonitrides, borides, oxides, oxynitrides, intermetallic compounds, or composite compounds thereof (S22) May be included. Thereby, the ceramic sintered compact containing the high pressure phase aluminum oxynitride containing the additive can be obtained.

  The step of producing the sintered body (S30) is performed at a pressure of 1 GPa or higher and a temperature of 1100 ° C. or higher and 2000 ° C. or lower using an ultrahigh pressure generator, or a pressure of 10 MPa or higher and a temperature of 800 ° C. or higher using a discharge plasma sintering apparatus. A step (S31) of sintering the high-pressure phase aluminum oxynitride powder or the second composite powder containing the high-pressure phase aluminum oxynitride at 1800 ° C. or lower may be included.

  According to another aspect of the present invention, there is provided a method for producing a ceramic sintered body comprising: a step of preparing a precursor from a starting material containing at least one of aluminum nitride and aluminum oxide (S11, S12); And a step of sintering at the same time as the phase transition to the phase to produce a sintered body (S32). Even in this manner, a composite powder containing high-pressure phase aluminum oxynitride can be produced.

  The step of producing the sintered body (S32) is to produce the sintered body simultaneously with the phase transition of the precursor to the high pressure phase at a pressure of 10 GPa or higher and a temperature of 1100 ° C. or higher and 2000 ° C. or lower using an ultrahigh pressure generator. The process of carrying out may be included.

  Next, examples of the present invention will be described.

  As a method for producing a ceramic sintered body according to the embodiment of the present invention, a product (sample) produced using the production method shown in FIG. 2 was evaluated.

(Evaluation sample)
First, 19 combinations of manufacturing conditions in step (S11), step (S13), and step (S21) in FIG. 2 were prepared, and products after step (S21) in each manufacturing method were analyzed (experiment). 1). In the step (S11), the mixing ratio of aluminum oxide (Al ₂ O ₃ ) and aluminum nitride (hAlN) is changed to Al ₂ O so that the composition ratio of oxygen atoms to nitrogen atoms contained in the aluminum oxynitride is 3 or more and 9 or less. ₃ : hAlN = 1: 1 to 7: 3 and the amount of oxygen adsorbed on the aluminum nitride so that the composition ratio of oxygen atoms to nitrogen atoms contained in the aluminum oxynitride is 3 or more and 9 or less Precursors were made in two ways of increasing. In the step (S13), the heating temperature is set in four conditions in the range of 1500 ° C. to 2100 ° C., and in the step (S21), as a method for producing high pressure phase aluminum oxynitride, a method of applying pressure using an ultrahigh pressure generator, A high-pressure phase aluminum oxynitride powder or a second composite powder containing a high-pressure phase aluminum oxynitride obtained after the 19-pattern step (S21) was prepared by combining the method using the aerosol deposition method and the respective conditions.

  After the evaluation in Experiment 1, the plurality of types of powders or composite powders described above were further subjected to step (S31) in FIG. 2 under the same conditions, and the finally obtained ceramic sintered body was analyzed (Experiment 2). . In the step (S22), TiN was used as an additive, and the above powder or composite powder and TiN were mixed at a ratio of 3: 1 to produce a molded body. In the step (S31), the compact was sintered at a pressure of 6 GPa and a temperature of 1300 ° C.

(Evaluation method of Experiment 1)
The amount of adsorbed oxygen was evaluated by an oxygen analyzer. Furthermore, the composition ratio of the mixture was evaluated using the intensity ratio of the main peak of X-ray diffraction (XRD). The composition ratio of aluminum oxynitride contained in the mixture was evaluated by EDX analysis.

  (Experiment 1 evaluation result)

Referring to Table 1, first, it was found that the amount of aluminum oxynitride produced varies greatly depending on the mixing ratio of aluminum oxide and aluminum nitride in the step (S11). Even if the mixing ratio of aluminum oxide to aluminum nitride is as small as Al ₂ O ₃ : hAlN = 1: 1 or as large as Al ₂ O ₃ : hAlN = 7: 3, oxynitriding in the mixture after step (S21) The ratio of aluminum was about 30% and was not generated sufficiently. On the other hand, when the mixing ratio of aluminum oxide and aluminum nitride was Al ₂ O ₃ : hAlN = 3: 2 or more and less than 7: 3, the ratio of aluminum oxynitride reached about 60%. Further, referring to Table 3, as a step (S11), the amount of adsorbed oxygen of aluminum nitride is increased so that the composition ratio of oxygen atoms to nitrogen atoms contained in aluminum oxynitride is 3 or more and 9 or less. When the body was manufactured, the powder was heat-treated so that the amount of adsorbed oxygen was 28 wt% or more and 33 wt% or less, and when fired in the same manner, the ratio of aluminum oxynitride reached about 60%. Further, it was found that when the amount of adsorbed oxygen was less than 28 wt% and more than 33 wt%, the ratio of aluminum oxynitride was reduced to about 30%. Therefore, it was found that in order to produce a sufficient amount of aluminum oxynitride, it is appropriate that the mixing ratio of the aluminum oxide powder and the aluminum nitride powder in the step (S11) is within the above range.

  Next, it was found that there is an appropriate range for the heating temperature in the step (S13). Even in the precursor mixed at the mixing ratio in the above range in the step (S11), when the heating temperature in the step (S13) is 1500 ° C., the ratio of aluminum oxynitride in the composite powder after the step (S21) is 2 However, it was not enough. On the other hand, when the heating temperature in the step (S13) was 2100 ° C., a sufficient amount of aluminum oxynitride was generated, but the composition of aluminum oxynitride was excessive nitrogen. That is, nitrogen is excessive, the spinel structure of aluminum oxynitride cannot be maintained, and the amount of aluminum nitride increases, so that a decrease in hardness is expected. In fact, in Experiment 2 below, it was confirmed that the ceramic sintered body produced under the conditions had a decrease in hardness. On the other hand, when the mixing ratio was within the above range in the step (S11) and the heating temperature was 1750 ° C., sufficient aluminum oxynitride could be produced, and the aluminum oxynitride did not become excessive in nitrogen.

  Next, in the step (S21), it was found that a sufficient amount of aluminum oxynitride was generated by adopting a method in which the precursor was pressurized with a shock wave having a pressure of 10 GPa or more. On the other hand, when the method of sintering the precursor using a multi-anvil apparatus was employed, the amount of aluminum oxynitride produced varied greatly depending on the sintering temperature.

  When the sintering temperature is 1100 ° C., a sufficient amount of aluminum oxynitride cannot be generated, and aluminum oxide and aluminum nitride exist in the mixture while maintaining the mixing ratio in the step (S11). On the other hand, at a sintering temperature of 2100 ° C., a sufficient amount of aluminum oxynitride was not generated, and nitrogen was desorbed from the entire mixture. In other words, it was considered that the composition of aluminum oxynitride was insufficient in nitrogen, and the amount of aluminum nitride in the mixture was extremely small, and conversion to aluminum oxide occurred.

  When the sintering temperature was 1750 ° C. and the pressure was 10 GPa or more, a sufficient amount of aluminum oxynitride could be generated. When the sintering temperature was 1750 ° C. and the pressure was 9 GPa, sufficient aluminum oxynitride was generated, and the composition ratio of aluminum oxynitride was appropriate.

  Note that the composition of the aluminum oxynitride was oxygen atom: nitrogen atom = 3: 2 to 9: 1 under the condition that the aluminum oxynitride was sufficiently manufactured.

(Evaluation method of Experiment 2)
The Vickers hardness of the ceramic sintered body was calculated from the indentation obtained by indenting a diamond indenter with a test load of 10 kgf. Furthermore, the ceramic sintered body was cut with a laser to produce a cutting tool having a nose R of 0.8 mm at the tip, and a cutting test was performed. In the cutting test, S45C steel was used as a workpiece, and the amount of wear on the flank of the cutting tool after cutting the workpiece made of S45C for 1 km was measured. The cutting conditions were a cutting speed of 400 m / min, a cutting amount of 0.2 mm, a feed amount per rotation of 0.1 mm / rev, and no cutting oil.

When a cutting tool made of general aluminum oxide Al ₂ O ₃ and aluminum oxynitride (atmospheric pressure phase aluminum oxynitride) not subjected to the step (S21) was evaluated by the above evaluation method, Al ₂ O ₃ The resulting cutting tool had a Vickers hardness of 2200 Hv, and the chipping occurred in the cutting test. On the other hand, the cutting tool made of aluminum oxynitride that was not subjected to the above step (S21) had Vickers hardness of 1600 Hv and a defect occurred in the cutting test.

  (Evaluation result of Experiment 2)

  The evaluation result of Experiment 2 will be described with reference to Table 4. The ceramic sintered body obtained from the mixture in which aluminum oxynitride was not sufficiently generated in Experiment 1 had a Vickers hardness of 2200 Hv or less, and sufficient hardness was not obtained. Also, a ceramic sintered body obtained from a mixture in which aluminum oxynitride has been sufficiently produced but the nitrogen atoms contained in the aluminum oxynitride is excessive (oxygen atoms: nitrogen atoms = 3: 2) is also pickers. A hardness of 2200 Hv was not sufficient. Furthermore, it was shown that these ceramic sintered bodies having insufficient hardness have a large flank wear amount of 100 μm or more in the cutting test, and are not suitable as materials for cutting tools because of the occurrence of defects. In particular, a cutting tool using a ceramic sintered body obtained from a mixture in which the composition of aluminum oxynitride was insufficient in nitrogen was lost during the cutting test. From this result, it was shown that the composition ratio of oxygen atoms to nitrogen atoms contained in aluminum oxynitride is preferably 3 or more and 9 or less.

  In the step (S21), the ceramic sinter obtained by using the multi-anvil apparatus and sintering the precursor at a pressure of 9 GPa and a temperature of 1750 ° C. has a sufficient amount of aluminum oxynitride generated. Despite this, the Vickers hardness was as low as 1980 Hv. That is, it is presumed that the phase transition to the high-pressure phase aluminum oxynitride did not proceed sufficiently due to insufficient pressure during sintering, or that the phase transformation to the normal pressure phase aluminum oxynitride occurred. Therefore, in the method of sintering using a multi-anvil apparatus at a process (S21), it was shown that it is preferable that a pressure shall be 10 GPa or more.

  From Example 1 above, a precursor having a molar ratio of aluminum oxide to aluminum nitride of 3/2 or more and 7/3 or less is generated, and the precursor is fired at a heating temperature of 1600 ° C. or more and 2000 ° C. or less. Can be produced at a pressure of 10 GPa or more, at a temperature of 1100 ° C. or more and 2000 ° C. or less, or by instantaneous pressurization with a shock wave of 10 GPa or more of pressure, and a material for a cutting tool having a higher hardness and longer life than conventional aluminum oxide or aluminum oxynitride It has been shown. At this time, it was confirmed that the composition ratio of oxygen atoms to nitrogen atoms contained in the aluminum oxynitride was preferably 3 or more and 9 or less.

Next, Example 2 will be described.
In this example, the effect of the additive added to the composite powder containing aluminum oxynitride obtained in step (S21) in step (S22) of FIG. 2 was evaluated. That is, at least one of Group 4, Group 5, Group 6 transition metal, or aluminum, silicon, boron, or a nitride, carbide, carbonitride, boride, or intermetallic compound thereof. A sintered body was prepared by mixing and evaluated. Moreover, in the manufacturing method of this invention shown in FIG. 2, the process (S22) was not included but the sintered compact produced without adding an additive was also evaluated.

(Evaluation sample)
First, a composite powder containing high-pressure phase aluminum oxynitride was produced by a method in which the mixture produced under a single condition in step (S11) and step (S13) was pressurized with a shock wave in step (S21). A _second material prepared by adding TiN, ZrN, HfN, VN, NbN, TaN, CrN, MoN, WN, TiC, and TiB ₂ as an additive to the aluminum oxynitride: additive = 7: 3 ratio. And a composite powder prepared without adding an additive were prepared. This was sintered in step (S31) to produce a ceramic sintered body. In addition, with respect to the 2nd composite powder which added TiN, 10 types of ceramic sintered compacts which changed the use equipment, pressure conditions, and sintering temperature conditions in the process (S31) were produced, and compared.

(Evaluation method)
The same items were evaluated by the same method as in Example 1. That is, the composition ratio of the composite powder obtained after the step (S21) and the composition ratio of aluminum oxynitride contained in the composite powder were evaluated. Further, the Vickers hardness of the ceramic sintered body and the wear amount of the flank in the cutting test when the cutting tool was used were evaluated.

  (Evaluation results)

  Table 5 shows the evaluation results when the method of applying pressure by shock waves in the step (S21) is adopted, and Table 6 shows the evaluation results when the method of sintering using the multi-anvil apparatus is adopted. In any method, when any one of the above additives is added, the Vickers hardness is as high as 2400 Hv or higher, and the wear amount of the flank in the cutting test is 100 μm or less, which is suitable as a cutting material. Indicated. Furthermore, it was confirmed that the Vickers hardness and the wear amount had the same performance even when no additive was added.

  However, in the step (S31), when a method of sintering using a belt device is adopted and the sintering conditions are set to a low temperature of 900 ° C. or a high temperature of 2200 ° C., the Vickers hardness of the obtained ceramic sintered body is , Both were 2200 Hv or less, and defects occurred in the cutting test. If the temperature is not sufficiently high as a sintering condition, the sintering is insufficient and the hardness is insufficient. On the other hand, if the sintering temperature is too high, nitrogen is desorbed and converted to aluminum oxide.

  Therefore, it was shown that the sintering conditions when the method of sintering using an ultra-high pressure generator in the step (S31) is adopted are preferably a pressure of 1 GPa or more and a temperature of 1100 ° C. or more and 2000 ° C. or less.

  On the other hand, when a method of sintering using a discharge plasma sintering apparatus is adopted and the sintering conditions are a low temperature of 700 ° C., a high temperature of 1900 ° C., or a low pressure of 5 MPa, the Vickers of the obtained ceramic sintered body is used. The hardness was 2000 Hv or less in all cases, and the wear amount in the cutting test was 100 μm or more. If the temperature is not sufficiently high as a sintering condition, the sintering is insufficient and the hardness is insufficient. On the other hand, if the sintering temperature is too high, nitrogen is desorbed and converted to aluminum oxide.

  In this example, a ceramic sintered body manufactured using the manufacturing method shown in FIG. 2 and a ceramic sintered body manufactured using the manufacturing method shown in FIG. 3 were evaluated.

(Evaluation sample)
Referring to FIG. 2, the precursor was prepared by mixing the aluminum oxide powder and the aluminum nitride powder prepared in step (S11) with additives in step (S11). As in Example 1, the mixing ratio of aluminum oxide and aluminum nitride was Al ₂ O ₃ : hAlN = 1: 1 to 7: 3 in four conditions, and the additives were TiN, ZrN, 11 types of HfN, VN, NbN, TaN, CrN, MoN, WN, TiC, TiB ₂ were prepared, and the ratio of the aluminum oxide powder, the aluminum nitride powder, and the additive prepared in the step (S11) was 7: 3. Precursors were made as proportions. Thereafter, the ceramic sintered body was produced under a single condition in each of the step (S13), the step (S21), and the step (S31). In the step (S13), the precursor is fired at a heating temperature of 1750 ° C., in the step (S21), the precursor is pressurized by a shock wave having a pressure of 15 GPa and a pressurization time of 50 μs, and in the step (S31), the pressure is 6 GPa and the heating temperature is 1300. The composite powder containing the high pressure phase aluminum oxynitride was sintered at ° C. Thus, the ceramic sintered compact manufactured using the manufacturing method shown in FIG. 2 was prepared.

  In addition, referring to FIG. 3, after preparing the precursor, sintering was performed using a multi-anvil apparatus at a pressure of 10 GPa and a temperature of 1750 ° C., and the phase transition to high-pressure phase aluminum oxynitride and the sintering were performed simultaneously. It was. Thus, the ceramic sintered compact manufactured using the manufacturing method shown in FIG. 3 was prepared.

(Evaluation method)
For the ceramic sintered body manufactured using the manufacturing method shown in FIG. 2, the same items were evaluated in the same manner as in Example 1 and Example 2. That is, the composition ratio of the composite powder obtained after the step (S21) and the composition ratio of aluminum oxynitride contained in the composite powder were evaluated. Further, the Vickers hardness of the ceramic sintered body and the wear amount of the flank in the cutting test when the cutting tool was used were evaluated.

  For the ceramic sintered body manufactured using the manufacturing method shown in FIG. 3, the composition ratio of the ceramic sintered body obtained after the step (S32) and the composition of the aluminum oxynitride contained in the ceramic sintered body The ratio was evaluated. Further, the Vickers hardness of the ceramic sintered body and the wear amount of the flank in the cutting test when the cutting tool was used were evaluated.

  (Evaluation results)

With reference to Table 7, the evaluation results of this example will be described. First, it was found that the mixing ratio of the aluminum oxide powder and the aluminum nitride powder in the step (S11) was preferably Al ₂ O ₃ : hAlN = 3: 2 or more and less than 7: 3, as in Example 1. . That is, within the above range, a sufficient amount of aluminum oxynitride can be produced, and the finally obtained ceramic sintered body has a high hardness of Vickers hardness of 2400 Hv or more, and a flank in a cutting test when used as a cutting tool. The amount of wear was 100 μm or less, which was a good result. On the other hand, outside the above range, a sufficient amount of aluminum oxynitride was not produced, and the finally obtained ceramic sintered body had a Vickers hardness of 2400 Hv or less, and the chip was missing in the cutting test when it was used as a cutting tool. Therefore, it was shown that it is not suitable as a material for cutting tools.

  As for the additive, any of the 11 types used in this example was used as a precursor with the mixing ratio of the aluminum oxide powder and the aluminum nitride powder within the above range, and the precursor and additive When the above mixture ratio is used, the finally obtained ceramic sintered body has a high hardness of Vickers hardness of 2400 Hv or more, and the wear amount of the flank in the cutting test when used as a cutting tool is 100 μm or less. It was.

  Note that the aluminum oxynitride manufactured in this example has a higher composition ratio of nitrogen atoms than the aluminum oxynitride evaluated in Example 1 and Example 2. In the manufacturing method shown in FIG. 2, nitride is used as an additive, and this is mixed with the precursor before the step (S13) and step (S21), so that the additive has good dispersibility. This is probably because the taken-in high-pressure phase aluminum oxynitride could be obtained. On the other hand, in the manufacturing method shown in FIG. 3, by using a nitride as an additive and mixing it with the precursor before the step (S32), the high-pressure phase in which the additive is incorporated with good dispersibility is used. This is probably because aluminum oxynitride could be obtained.

  Moreover, after producing the precursor, sintering was performed at a pressure of 10 GPa and a temperature of 1750 ° C. using a multi-anvil apparatus, and the phase transition to high-pressure phase aluminum oxynitride and the sintering were simultaneously performed. It was confirmed that the ceramic sintered body manufactured using the method had the same performance as the ceramic sintered body manufactured using the manufacturing method shown in FIG. 2 in terms of Vickers hardness and wear amount.

  As described above, the embodiments and examples of the present invention have been described. However, it should be understood that the embodiments disclosed herein are illustrative and non-restrictive in every respect. The scope of the present invention is defined by the terms of the claims, and is intended to include any modifications within the scope and meaning equivalent to the terms of the claims.

  The ceramic sintered body of the present invention is particularly advantageously applied as a cutting tool material.

Claims (8)

Including aluminum oxynitride,
Vickers hardness is Ri Der more 3800Hv following 2400Hv,
The composition ratio of oxygen atoms to nitrogen atoms contained in the aluminum oxynitride is 3 or more and 9 or less,
The intensity ratio of the main peak of X-ray diffraction of the aluminum oxynitride is 50% or more,
Ceramic sintered body that does not contain silicon carbide .   Group 4, Group 5, Group 6 transition element, or aluminum, silicon, boron, or nitrides, carbides, carbonitrides, borides, oxides, oxynitrides, intermetallic compounds, or The ceramic sintered body according to claim 1, further comprising at least one of the composite compounds.   The ceramic sintered body according to claim 1 or 2, further comprising at least one of aluminum nitride and aluminum oxide.   A tool using the ceramic sintered body according to claim 1. A precursor is prepared from a starting material containing at least one of aluminum nitride and aluminum oxide, and an atmospheric pressure phase aluminum oxynitride powder or a first composite powder containing atmospheric pressure phase aluminum oxynitride is produced from the precursor. And a process of
A step of producing a high pressure phase aluminum oxynitride powder or a second composite powder containing high pressure phase aluminum oxynitride from the normal pressure phase aluminum oxynitride powder or the first composite powder containing normal pressure phase aluminum oxynitride. When,
A step of producing a sintered body by sintering the high-pressure phase aluminum oxynitride powder or the second composite powder containing the high-pressure phase aluminum oxynitride ,
When the starting material includes the aluminum nitride and the aluminum oxide, the mixing ratio of the aluminum oxide and the aluminum nitride in the starting material is 3: 2 or more and less than 7: 3, and the starting material is the nitriding When only aluminum is included, the adsorbed oxygen amount of the aluminum nitride is 28 wt% or more and 33 wt% or less,
In the step of producing the atmospheric pressure phase aluminum oxynitride powder or the first composite powder containing the atmospheric pressure phase aluminum oxynitride, the composition ratio of oxygen atoms to nitrogen atoms contained in the high pressure phase aluminum oxynitride is 3 or more. The step of producing the precursor so as to be 9 or less, and the precursor is fired under the conditions of a heating temperature of 1600 ° C. or more and 2000 ° C. or less, whereby the normal pressure phase aluminum oxynitride powder or the normal pressure phase acid Producing the first composite powder containing aluminum nitride,
The step of producing the high-pressure phase aluminum oxynitride powder or the second composite powder containing the high-pressure phase aluminum oxynitride instantaneously generates the atmospheric pressure phase oxynitride by a shock wave having a pressure of 15 GPa or more and a pressurization time of 50 μsec or less. Pressurizing the first composite powder containing aluminum powder or atmospheric pressure phase aluminum oxynitride, and using the ultrahigh pressure generator, the atmospheric pressure phase aluminum oxynitride at a pressure of 10 GPa or more and a temperature of 1200 ° C to 2000 ° C Using the step of pressurizing the first composite powder containing powder or atmospheric pressure phase aluminum oxynitride and the aerosol deposition method, the carrier gas flow rate is 1 SLM and the particle velocity collides with the substrate at 150 m / s or more. Including one selected from the group consisting of:
The step of producing the sintered body is performed at a pressure of 1 GPa or more and a temperature of 1100 ° C. or more and 2000 ° C. or less using an ultrahigh pressure generator, or a pressure of 10 MPa or more and a temperature of 800 ° C. or more and 1800 ° C. or less using a discharge plasma sintering apparatus. A method for producing a ceramic sintered body, comprising the step of sintering the high-pressure phase aluminum oxynitride powder or the second composite powder containing the high-pressure phase aluminum oxynitride . In the step of producing the normal pressure phase aluminum oxynitride powder or the first composite powder containing the normal pressure phase aluminum oxynitride,
At least one of the precursor, the atmospheric pressure phase aluminum oxynitride powder, and the first composite powder includes a transition metal of Group 4, Group 5, or Group 6, or aluminum, silicon, boron or nitrides thereof, carbides, carbonitrides, borides, oxides, oxynitrides, intermetallic compounds, or of their complex compounds, including the step of adding at least one, according to claim 5 Of manufacturing a ceramic sintered body. The step of preparing the high-pressure phase aluminum oxynitride powder or the second composite powder containing the high-pressure phase aluminum oxynitride includes
The high-pressure phase aluminum oxynitride powder or the second composite powder containing the high-pressure phase aluminum oxynitride includes a Group 4, Group 5, Group 6 transition metal, or aluminum, silicon, boron, or their The ceramic firing according to claim 5, further comprising adding at least one of nitride, carbide, carbonitride, boride, oxide, oxynitride, intermetallic compound, or a composite compound thereof. A method for producing a knot. Preparing a precursor from a starting material containing at least one of aluminum nitride and aluminum oxide;
A step of sintering the precursor simultaneously with the phase transition to a high-pressure phase, and preparing a sintered body,
The step of producing the sintered body, the pressure 10GPa or more using a high-pressure apparatus, temperature 1 2 00 ° C. or higher 2000 ° C. or less, the processing time of 20 minutes or more, at the same time the precursor phase transition into the high-pressure phase the viewing including the step of producing a sintered body,
In the step of preparing the precursor, the precursor is produced such that the composition ratio of oxygen atoms to nitrogen atoms contained in the high-pressure phase is 3 or more and 9 or less .

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