JP6409441B2 - Cubic sialon, sintered body, tool including sintered body, method for manufacturing cubic sialon, and method for manufacturing sintered body - Google Patents

Description

  The present invention relates to a cubic sialon, a sintered body, a tool including a sintered body, a method for producing a cubic sialon, and a method for producing a sintered body.

  Sialon (hereinafter also referred to as SiAlON) has a structure in which aluminum and oxygen are dissolved in silicon nitride. Sialons are classified according to crystal structure into α-type and β-type sialons belonging to the hexagonal system. Furthermore, it is known that cubic sialon belonging to a cubic system can be synthesized by instantaneously pressurizing β-sialon with a shock wave. Since cubic sialon is a high-pressure phase of β-sialon, it has higher density and higher hardness than β-sialon.

  Since a sintered body using sialon has a characteristic of low reactivity with a workpiece, research as a cutting tool material has been advanced.

  For example, Patent Document 1 (Japanese Patent Application Laid-Open No. 2011-256067) discloses a sintered body containing cubic sialon, β-sialon, and at least one of a first compound and a second compound, The one compound is at least one element selected from the group consisting of iron, cobalt, nickel, Group 4a element, Group 5a element, and Group 6a element of the periodic table, and the second compound includes At least one element selected from the group consisting of Group 4a elements, Group 5a elements, and Group 6a elements, and at least one element selected from the group consisting of carbon, nitrogen and boron A sintered body which is a compound is disclosed.

  Patent Document 2 (Japanese Patent Application Laid-Open No. 2013-234093) discloses a sintered body including sialon-based particles including at least one of α-type sialon and β-type sialon and cubic sialon (γ-type sialon). ing.

JP 2011-256067 A JP 2013-234093 A

  Since the techniques of Patent Document 1 and Patent Document 2 include high-hardness cubic sialon and α-sialon, β-sialon, first compound, second compound, etc. having lower hardness than cubic sialon, There is a problem that the wear resistance of the bonded body is lowered.

  Therefore, this purpose is to improve the wear resistance and fracture resistance of the sintered body when used as a material of the sintered body, cubic sialon, sintered body containing cubic sialon, sintered It is an object to provide a tool including a body, a method of manufacturing a cubic sialon, and a method of manufacturing a sintered body.

A cubic sialon according to one embodiment of the present invention has the following formula (1):
M _x Si _(6-xy) Al _y O _y N _(8-y) (1)
(In the formula (1), M is composed of calcium, strontium, barium, scandium, yttrium, lanthanoid, manganese, iron, cobalt, nickel, copper, Group 4 element, Group 5 element and Group 6 element of the periodic table. A first metal including at least one selected from the group, and a relationship of 0.01 ≦ x ≦ 2, 0.01 ≦ y ≦ 4.2, and 1.79 ≦ (6-xy) ≦ 5.98 Meet)
It is a cubic sialon represented by

  A sintered body according to one embodiment of the present invention is a sintered body containing the above cubic sialon in an amount of 20% by volume to 100% by volume.

The cutting tool which concerns on 1 aspect of this invention is a cutting tool provided with said sintered compact.
A method for producing a cubic sialon according to one embodiment of the present invention includes calcium, strontium, barium, scandium, yttrium, lanthanoid, manganese, iron, cobalt, nickel, copper, a Group 4 element and a Group 5 element in the periodic table. And a step of preparing a first particle group containing at least one selected from the group consisting of a group 6 element, silicon and aluminum, heat-treating the first particle group, the first metal, silicon, A step of producing a second particle group containing aluminum, oxygen, and nitrogen; and a step of producing a cubic sialon by treating the second particle group by an impact compression method or a static pressure synthesis method. Sialon has the following formula (1)
M _x Si _(6-xy) Al _y O _y N _(8-y) (1)
(In the formula (1), M is composed of calcium, strontium, barium, scandium, yttrium, lanthanoid, manganese, iron, cobalt, nickel, copper, Group 4 element, Group 5 element and Group 6 element of the periodic table. A first metal including at least one selected from the group, and satisfying a relationship of 0.01 ≦ y ≦ 4.2 and 1.79 ≦ (6-xy) ≦ 5.98) This is a method for producing crystal sialon.

A method for producing a sintered body according to one embodiment of the present invention includes calcium, strontium, barium, scandium, yttrium, lanthanoid, manganese, iron, cobalt, nickel, copper, a group 4 element in the periodic table, a group 5 element, and Preparing a first particle group including a first metal containing at least one selected from the group consisting of Group 6 elements, silicon and aluminum and heat-treating the first particle group; A step of producing a second particle group containing oxygen and nitrogen, a step of treating the second particle group by an impact compression method or a static pressure synthesis method to produce a cubic sialon, and 20 volumes of cubic sialon %, And a step of preparing a third particle group including 100% by volume or less and a step of obtaining a sintered body by sintering the third particle group. The cubic sialon is represented by the following formula (1):
M _x Si _(6-xy) Al _y O _y N _(8-y) (1)
(In the formula (1), M is composed of calcium, strontium, barium, scandium, yttrium, lanthanoid, manganese, iron, cobalt, nickel, copper, Group 4 element, Group 5 element and Group 6 element of the periodic table. A first metal containing at least one selected from the group, and satisfying the relationship of 0.01 ≦ y ≦ 4.2 and 1.79 ≦ (6-xy) ≦ 5.98) It is a manufacturing method of a zygote.

  According to the above aspect, the cubic sialon capable of improving the wear resistance and fracture resistance of the sintered body when used as the material of the sintered body, the sintered body containing the cubic sialon, and the sintered body A tool including a body, a method of manufacturing a cubic sialon, and a method of manufacturing a sintered body can be provided.

It is a flowchart which shows the manufacturing method of the cubic sialon which concerns on 1 aspect of this invention. It is a flowchart which shows the manufacturing method of the sintered compact which concerns on 1 aspect of this invention.

[Description of Embodiment of the Present Invention]
First, embodiments of the present invention will be listed and described.

(1) A cubic sialon according to one embodiment of the present invention has the following formula (1):
M _x Si _(6-xy) Al _y O _y N _(8-y) (1)
(In the formula (1), M is composed of calcium, strontium, barium, scandium, yttrium, lanthanoid, manganese, iron, cobalt, nickel, copper, Group 4 element, Group 5 element and Group 6 element of the periodic table. A first metal including at least one selected from the group, and a relationship of 0.01 ≦ x ≦ 2, 0.01 ≦ y ≦ 4.2, and 1.79 ≦ (6-xy) ≦ 5.98 Meet)
It is a cubic sialon represented by

  The cubic sialon according to one embodiment of the present invention can improve the wear resistance of the sintered body when used as a material of the sintered body. The reason is presumed as follows. The cubic sialon represented by the formula (1) includes cubic sialon, calcium, strontium, barium, scandium, yttrium, lanthanoid, manganese, iron, cobalt, nickel, copper, a group 4 element of the periodic table, Since it is obtained by dissolving a first metal containing at least one selected from the group consisting of Group 5 elements and Group 6 elements, residual stress is imparted in the cubic sialon particles. Therefore, the cubic sialon according to one embodiment of the present invention has a hardness higher than that of a conventional cubic sialon in which the first metal is not dissolved, and further has improved crack propagation resistance. Therefore, when the cubic sialon according to one embodiment of the present invention is used as a material for a sintered body, the sintered body is considered to exhibit excellent wear resistance and fracture resistance against mechanical abrasion.

  The cubic sialon according to one embodiment of the present invention can improve the fracture resistance of the sintered body when used as a material of the sintered body. The reason is presumed as follows. Since the first metal is uniformly dispersed in the cubic sialon particles, resistance to crack propagation in the particles can be increased. Therefore, the cubic sialon according to one embodiment of the present invention has a crack propagation resistance higher than that of a conventional cubic sialon in which the first metal is not dispersed. Therefore, when the cubic sialon according to one embodiment of the present invention is used as a material for a sintered body, the sintered body is considered to exhibit excellent fracture resistance against intermittent cutting.

  (2) It is preferable that the cubic sialon includes 0.01% by mass to 5% by mass of the first metal simple substance. According to this, the defect resistance improvement effect can be obtained by the first metal uniformly dispersed in the cubic sialon particles.

  (3) The sintered body according to one embodiment of the present invention includes 20% by volume or more and 100% by volume or less of the cubic sialon according to (1) or (2). The sintered body can have excellent wear resistance and fracture resistance against mechanical abrasion.

  (4) The sintered body is a sintered body including the cubic sialon according to the above (1) or (2), and one or both of the second metal and the first compound, The second metal includes at least one selected from the group consisting of manganese, iron, cobalt, nickel and copper, and the first compound is aluminum, boron, silicon, manganese, iron, cobalt, nickel, copper, calcium, At least one first element selected from the group consisting of yttrium, Group 4 elements, Group 5 elements and Group 6 elements in the periodic table, and at least one selected from the group consisting of carbon, nitrogen, oxygen and boron It is preferable to contain at least one compound composed of the second element.

  The second metal and the first compound serve as a binder phase in the sintered body. Therefore, when the sintered body contains one or both of the second metal and the first compound, it can have excellent wear resistance and fracture resistance against mechanical abrasion.

  (5) The cutting tool which concerns on 1 aspect of this invention is a cutting tool provided with the sintered compact as described in said (3) or (4).

  Since the sintered body is excellent in wear resistance and fracture resistance, a cutting tool using the sintered body is also excellent in wear resistance and fracture resistance. Therefore, the cutting tool according to one embodiment of the present invention can have a longer life as compared with the conventional cutting tool.

(6) At least one selected from the group consisting of calcium, strontium, barium, scandium, yttrium, lanthanoid, manganese, iron, cobalt, nickel, copper, Group 4 element, Group 5 element and Group 6 element of the periodic table Preparing a first particle group including a first metal including seeds, silicon, and aluminum; and heat-treating the first particle group to form second particles including the first metal, silicon, aluminum, oxygen, and nitrogen. A step of producing a group, and a step of producing a cubic sialon by treating the second particle group by an impact compression method or a static pressure synthesis method, wherein the cubic sialon is represented by the following formula (1):
M _x Si _(6-xy) Al _y O _y N _(8-y) (1)
(In the formula (1), M is composed of calcium, strontium, barium, scandium, yttrium, lanthanoid, manganese, iron, cobalt, nickel, copper, Group 4 element, Group 5 element and Group 6 element of the periodic table. A first metal including at least one selected from the group, and satisfying a relationship of 0.01 ≦ y ≦ 4.2 and 1.79 ≦ (6-xy) ≦ 5.98) This is a method for producing crystal sialon.

  When the cubic sialon thus obtained is used as a material for a sintered body, the wear resistance and fracture resistance of the sintered body can be improved.

(7) A method for manufacturing a sintered body according to one embodiment of the present invention includes calcium, strontium, barium, scandium, yttrium, lanthanoid, manganese, iron, cobalt, nickel, copper, a Group 4 element of the periodic table, a fifth Preparing a first particle group including a first metal including at least one selected from the group consisting of a group element and a group 6 element, silicon and aluminum, heat-treating the first particle group, Producing a second particle group containing metal, silicon, aluminum, oxygen and nitrogen; and treating the second particle group by an impact compression method or a static pressure synthesis method to produce a cubic sialon; A step of preparing a third particle group containing 20% by volume or more and 100% by volume or less of the cubic sialon; and a step of sintering the third particle group to obtain a sintered body. Type sialon is represented by the following formula (1)
M _x Si _(6-xy) Al _y O _y N _(8-y) (1)
(In the formula (1), M is composed of calcium, strontium, barium, scandium, yttrium, lanthanoid, manganese, iron, cobalt, nickel, copper, Group 4 element, Group 5 element and Group 6 element of the periodic table. A first metal containing at least one selected from the group, and satisfying the relationship of 0.01 ≦ y ≦ 4.2 and 1.79 ≦ (6-xy) ≦ 5.98) It is a manufacturing method of a zygote.

  The sintered body thus obtained can exhibit excellent wear resistance and fracture resistance against mechanical abrasion.

  (8) In the method for manufacturing a sintered body, the third particle group includes the cubic sialon, and one or both of a second metal and a first compound, and the second metal is manganese. And at least one selected from the group consisting of iron, cobalt, nickel and copper, wherein the first compound is aluminum, boron, silicon, manganese, iron, cobalt, nickel, copper, calcium, yttrium From at least one first element selected from the group consisting of Group 4 elements, Group 5 elements and Group 6 elements, and at least one second element selected from the group consisting of carbon, nitrogen, oxygen and boron It is preferable to contain at least one compound.

The second metal and the first compound serve as a binder phase in the sintered body. Therefore, by producing a sintered body using one or both of the second metal and the first compound, the obtained sintered body has excellent wear resistance and fracture resistance against mechanical abrasion. Can have sex.
[Details of the embodiment of the present invention]
Embodiments of the present invention will be described in detail below. In addition, this invention is not limited to these illustrations, is shown by the claim, and intends that all the changes within the meaning and range equivalent to a claim are included.

  In the present specification, “metal” is not limited to a single metal composed of one kind of metal element, and includes an alloy composed of two or more kinds of metal elements, unless otherwise specified. In the present specification, the “compound” refers to a compound composed of one or more metal elements and one or more non-metal elements. Note that examples of the non-metallic element include carbon, nitrogen, oxygen, and boron.

  When the atomic ratio is not particularly defined in the chemical formulas described in the present specification, the atomic ratio of each element is not necessarily equal, and all conventionally known atomic ratios are included. For example, when written as TiN, the atomic ratio of Ti and N includes 1: 1, and includes 2: 1, 1: 0.95, 1: 0.9, and the like.

<First Embodiment>
The cubic sialon according to the first embodiment has the following formula (1):
M _x Si _(6-xy) Al _y O _y N _(8-y) (1)
(In the formula (1), M is composed of calcium, strontium, barium, scandium, yttrium, lanthanoid, manganese, iron, cobalt, nickel, copper, Group 4 element, Group 5 element and Group 6 element of the periodic table. A first metal including at least one selected from the group, and a relationship of 0.01 ≦ x ≦ 2, 0.01 ≦ y ≦ 4.2, and 1.79 ≦ (6-xy) ≦ 5.98 Meet)
It is represented by

  The cubic sialon represented by the formula (1) is greatly different from the conventional cubic sialon.

Conventional cubic sialon has, for example, a crystal structure similar to that of spinel, which is a mineral belonging to a cubic system composed of magnesium aluminate (MgAl ₂ O ₃ ), and has the general formula Si _(6-x) Al _x O. _x N _(8−x) (0 <x ≦ 4.2).

  On the other hand, the cubic sialon according to the first embodiment is a calcium (Ca), strontium (Sr), barium (Ba), scandium (Sc), yttrium (Y), in addition to the conventional cubic sialon. Selected from the group consisting of lanthanoids, manganese (Mn), iron (Fe), cobalt (Co), nickel (Ni), copper (Cu), group 4 elements, group 5 elements and group 6 elements of the periodic table It has a structure in which a first metal including at least one kind is dissolved.

  In this specification, lanthanoids include lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), promethium (Pm), samarium (Sm), europium (Eu), gadolinium (Gd), terbium ( Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb) and lutetium (Lu). In this specification, Group 4 elements of the periodic table include titanium (Ti), zirconium (Zr), and hafnium (Hf), and Group 5 elements include vanadium (V), niobium (Nb), and tantalum (Ta). Group 6 elements include chromium (Cr), molybdenum (Mo), and tungsten (W).

  The first metal has an atomic radius larger than that of silicon and aluminum. In the cubic sialon according to the present embodiment, since the first metal having an atomic radius different from that of silicon and aluminum is dissolved, residual stress is given in the particles. Accordingly, the cubic sialon has a hardness higher than that of the cubic sialon and further improves the crack propagation resistance. Therefore, when the cubic sialon is used as a material for the sintered body, it is considered that the sintered body exhibits excellent wear resistance and fracture resistance against mechanical abrasion.

The cubic sialon of the present embodiment has the following formula (1):
M _x Si _(6-xy) Al _y O _y N _(8-y) (1)
The relations 0.01 ≦ x ≦ 2, 0.01 ≦ y ≦ 4.2 and 1.79 ≦ (6-xy) ≦ 5.98 are satisfied.

  In the formula (1), when x is less than 0.01, the residual stress in the cubic sialon is insufficient, so that it is difficult to obtain an effect of improving the wear resistance. Moreover, x = 2 indicates the solid solution limit value of the first metal. The range of x is preferably 0.1 ≦ x ≦ 1.5, and more preferably 0.5 ≦ x ≦ 1.

  When y is less than 0.01, chemical stability and mechanical strength suitable for cutting are inferior. Moreover, y of 4.2 indicates the solid solution limit value of Al. The range of y is preferably 0.1 ≦ y ≦ 4, and more preferably 0.5 ≦ y ≦ 3.

  (6-xy) = 1.79 is the upper limit of substitution of Si. When the value of (6-xy) exceeds 5.98, chemical stability and mechanical strength suitable for cutting are inferior. The range of the value of (6-xy) is preferably 2 ≦ (6-xy) ≦ 5.5, more preferably 3 ≦ (6-xy) ≦ 5.

  The cubic sialon preferably contains 0.01% by mass to 5% by mass of the first metal simple substance. When the first metal uniformly dispersed in the cubic sialon particles is less than 0.01% by mass, the effect of increasing the fracture resistance is hardly observed. On the other hand, when the content is 5% by mass or more, the hardness of the sialon particles is lowered, so that the wear resistance against mechanical abrasion is lowered. The amount of the first metal element dispersed in the cubic sialon is preferably 0.05% by mass or more and 4% by mass or less, and more preferably 0.1% by mass or more and 3% by mass or less.

<Second Embodiment>
The sintered body according to the second embodiment includes 20% by volume or more and 100% by volume or less of the cubic sialon of the first embodiment. The sintered body can have excellent wear resistance and fracture resistance against mechanical abrasion.

  When the content of the cubic sialon in the sintered body is 20% by volume or more, the wear resistance and fracture resistance of the sintered body are improved. The content of cubic sialon in the sintered body is preferably 50% by volume to 100% by volume, more preferably 50% by volume to 90% by volume, and further preferably 50% by volume to 80% by volume.

  The sintered body is a sintered body including cubic sialon and one or both of the second metal and the first compound, and the second metal includes manganese, iron, cobalt, nickel, and copper. The first compound includes at least one selected from the group consisting of aluminum, boron, silicon, manganese, iron, cobalt, nickel, copper, calcium, yttrium, Group 4 elements and Group 5 elements of the periodic table And at least one compound consisting of at least one first element selected from the group consisting of Group 6 elements and at least one second element selected from the group consisting of carbon, nitrogen, oxygen and boron It is preferable.

  The 2nd metal and 1st compound in a sintered compact exist in the interface of adjacent cubic sialon, and play the role of a binder phase. Since the binder phase can firmly bond cubic sialons, the sintered body can have further excellent wear resistance and fracture resistance.

  Further, by including a binder phase in the sintered body, the sintered body can further have characteristics due to the binder phase in addition to characteristics due to the characteristics of the cubic sialon. Therefore, by appropriately adjusting the composition of the binder phase, the sintered body can flexibly meet each need required for various cutting conditions. For example, when the binder phase includes cubic boron nitride, the cubic boron nitride has an extremely high hardness. Therefore, the sintered body having the binder phase including the cubic boron nitride can have a high hardness.

  As the second metal, for example, one kind of metal such as manganese, iron, cobalt, nickel and copper, or an alloy containing these metals can be used. One type of the second metal may be used, or two or more types may be used in combination.

  As the first compound, for example, a carbide, nitride, oxide, or boride of the first element can be used.

Examples of the first element carbide include silicon carbide (SiC), titanium carbide (TiC), zirconium carbide (ZrC), hafnium carbide (HfC), vanadium carbide (VC), niobium carbide (NbC), and tantalum carbide (TaC). Chromium carbide (Cr ₃ C ₂ ), molybdenum carbide (Mo ₂ C), tungsten carbide (WC), and the like can be used.

Examples of the nitride of the first element include boron nitride (BN), aluminum nitride (AlN), silicon nitride (Si ₃ N ₄ ), titanium nitride (TiN), zirconium nitride (ZrN), hafnium nitride (HfN), and nitride Vanadium (VN), niobium nitride (NbN), tantalum nitride (TaN), chromium nitride (Cr ₂ N), molybdenum nitride (MoN), tungsten nitride (WN), 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 nitride hafnium (ZrHfN), Zirconium nitride Ni vanadium (ZrVN), zirconium niobium nitride (ZrNbN), zirconium tantalum nitride (ZrTaN), zirconium chromium chromium (ZrCrN), zirconium molybdenum molybdenum (ZrMoN), zirconium tungsten nitride (ZrWN), hafnium vanadium nitride (HfVN), hafnium nitride Niobium (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 nitride molybdenum (VMoN), vanadium tungsten nitride (VWN), niobium tantalum nitride (NbT) N), niobium chromium nitride (NbCrN), niobium molybdenum nitride (NbMoN), niobium tungsten nitride (NbWN), tantalum chromium nitride (TaCrN), tantalum molybdenum nitride (TaMoN), tantalum tungsten nitride (TaWN), chromium molybdenum nitride (CrMoN) , Chromium tungsten nitride (CrWN), and molybdenum nitride chromium (MoWN).

Examples of the oxide of the first element include silicon oxide (SiO ₂ ), aluminum oxide (Al ₂ O ₃ ), calcium oxide (CaO ₂ ), titanium oxide (TiO ₂ ), zirconium oxide (ZrO ₂ ), and 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 ), and tungsten oxide ( WO ₃₎ can be used.

As the boride of the first element, for example, silicon boride (SiB ₄ ), aluminum boride (AlB ₁₂ ), titanium boride (TiB ₂ ), zirconium boride (ZrB ₂ ), hafnium boride (HfB ₂ ), Vanadium boride (VB), niobium boride (NbB ₂ ), tantalum boride (TaB ₂ ), chromium boride (CrB ₂ ), molybdenum boride (MoB), and tungsten boride (WB) can be used.

1 type may be used for a 1st compound and it may use it in combination of 2 or more type.
The total content of the second metal and the first compound in the sintered body exceeds 0% by volume, preferably 50% by volume or less, more preferably 10% by volume or more and 50% by volume or less, and 20% by volume or more and 50% by volume. % Or less is more preferable. When the total content of the second metal and the first compound in the sintered body exceeds 0% by volume and is 50% by volume or less, the wear resistance and fracture resistance of the sintered body are improved.

<Third Embodiment>
The cutting tool according to the third embodiment is a tool using the sintered body according to the second embodiment. As described above, since the sintered body containing the cubic sialon represented by the above formula (1) is excellent in wear resistance and fracture resistance, a tool using the sintered body is also excellent in these characteristics. Become.

  Examples of the cutting tool according to the third embodiment 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.

  When the whole cutting tool consists of the said sintered compact, a cutting tool can be produced by processing a sintered compact into a desired shape. The sintered body can be processed by, for example, laser or wire discharge. Moreover, when a part of cutting tool consists of the said sintered compact, a cutting tool can be produced by joining a sintered compact to the desired position of the base | substrate which comprises a tool. 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.

<Fourth Embodiment>
A method for producing a cubic sialon according to the fourth embodiment will be described with reference to FIG.

The method for producing cubic sialon comprises calcium, strontium, barium, scandium, yttrium, lanthanoid, manganese, iron, cobalt, nickel, copper, Group 4 element, Group 5 element and Group 6 element in the periodic table. A step of preparing a first particle group containing a first metal containing at least one selected from the group, silicon, and aluminum (shown as S1 in FIG. 1; hereinafter, also referred to as “first particle group preparing step”) And a step of heat-treating the first particle group to produce a second particle group containing the first metal, silicon, aluminum, oxygen, and nitrogen (shown as S2 in FIG. 1). And a process of producing a cubic sialon by treating the second particle group by an impact compression method or a static pressure synthesis method (shown as S3 in FIG. 1). It provided with the also referred to) and the cubic sialon manufacturing process ". The cubic sialon has the following formula (1)
M _x Si _(6-xy) Al _y O _y N _(8-y) (1)
(In the formula (1), M is composed of calcium, strontium, barium, scandium, yttrium, lanthanoid, manganese, iron, cobalt, nickel, copper, Group 4 element, Group 5 element and Group 6 element of the periodic table. A first metal including at least one selected from the group, and satisfying the relationship of 0.01 ≦ y ≦ 4.2 and 1.79 ≦ (6-xy) ≦ 5.98).

(First particle group preparation step)
Referring to FIG. 1, in the first particle group preparation step (S1), calcium, strontium, barium, scandium, yttrium, lanthanoid, manganese, iron, cobalt, nickel, copper, Group 4 element of Periodic Table, Group 5 A first particle group including a first metal including at least one selected from the group consisting of an element and a group 6 element, silicon, and aluminum is prepared.

  The first particle group is a raw material particle group that is a raw material of cubic sialon. Of the first metal, silicon, aluminum, oxygen and nitrogen constituting the cubic sialon, the first metal, silicon and aluminum are supplied only from the first particle group. For this reason, the content ratio of the first metal, silicon and aluminum in the first particle group needs to be the same as the content ratio of the first metal, silicon and aluminum in the target cubic sialon. On the other hand, oxygen and nitrogen in the cubic sialon can be supplied from the first particle group and from the atmosphere (oxygen atmosphere, nitrogen atmosphere, etc.) in the subsequent process. For this reason, the content ratio of oxygen and nitrogen in the first particle group need not be the same as the content ratio of oxygen and nitrogen in the cubic sialon.

  The first particle group includes particles containing a first metal, particles containing silicon, and particles containing aluminum.

  As the particles containing the first metal, particles made of one kind of element constituting the first metal and particles made of two or more kinds of elements constituting the first metal can be used. Specifically, for example, calcium particles, strontium particles, barium particles, scandium particles, yttrium particles, manganese particles, iron particles, cobalt particles, nickel particles, copper particles, lanthanum particles, cerium particles, praseodymium particles, neodymium particles, promethium Particles, samarium particles, europium particles, gadolinium particles, terbium particles, dysprosium particles, holmium particles, erbium particles, thulium particles, ytterbium particles, lutetium particles, titanium particles, zirconium particles, hafnium particles, vanadium particles, niobium particles, tantalum particles, Chromium particles, molybdenum particles, tungsten particles, titanium zirconium (TiZr) particles, titanium hafnium (TiHf) particles, titanium vanadium (TiV) particles, titanium niobium (T Nb) particles, titanium tantalum (TiTa) particles, titanium chromium (TiCr) particles, titanium molybdenum (TiMo) particles, titanium tungsten (TiW) particles, zirconium hafnium (ZrHf) particles, zirconium vanadium (ZrV) particles, zirconium niobium (ZrNb) ) Particles, zirconium tantalum (ZrTa) particles, zirconium chrome (ZrCr) particles, zirconium molybdenum (ZrMo) particles, zirconium tungsten (ZrW) particles, hafnium vanadium (HfV) particles, hafnium niobium (HfNb) particles, hafnium tantalum (HfTa particles) ), Hafnium chromium (HfCr) particles, hafnium molybdenum (HfMo) particles, hafnium tungsten (HfW) particles, vanadium niobium (VNb) particles, vanadium Mutantalum (VTa) particles, vanadium chromium (VCr) particles, vanadium molybdenum (VMo) particles, vanadium tungsten (VW) particles, niobium tantalum (NbTa) particles, niobium chromium (NbCr) particles, niobium molybdenum (NbMo) particles, niobium tungsten ( NbW) particles, tantalum chromium (TaCr) particles, tantalum molybdenum (TaMo) particles, tantalum tungsten (TaW) particles, chromium molybdenum (CrMo) particles, chromium tungsten (CrW) particles, molybdenum chromium (MoW) particles can be used. .

  As the particles containing the first metal, oxide, nitride, or oxynitride particles of an element constituting the first metal can also be used.

Examples of the oxide of the element constituting the first metal include calcium oxide (CaO), strontium oxide (SrO), barium oxide (BaO), scandium oxide (Sc ₂ O ₃ ), and yttrium oxide (Y ₂ O ₃ ). , Lanthanum oxide (La ₂ O ₃ ), cerium oxide (CeO ₂ ), praseodymium oxide (Pr ₂ O ₃ ), neodymium oxide (Nd ₂ O ₃ ), promethium oxide (Pm ₂ O ₃ ), samarium oxide (Sm ₂ O ₃ ), europium oxide (Eu ₂ O ₃ ), gadolinium oxide (Gd ₂ O ₃ ), terbium oxide (Tb ₂ O ₃ ), dysprosium oxide (Dy ₂ O ₃ ), holmium oxide (Ho ₂ O ₃ ), erbium oxide _(Er 2 _O 3), thulium oxide _{(Tm 2 O} 3), ytterbium oxide _{(Yb 2 O} 3), oxide Le Lithium _{(Lu 2 O} 3), titanium oxide _(TiO 2), zirconium oxide _(ZrO 2), hafnium oxide _(HfO 2), vanadium oxide _{(V 2 O} 5), niobium oxide (NbO), tantalum oxide _(Ta 2 O ₅ ), chromium oxide (Cr ₂ O ₃ ), molybdenum oxide (MoO ₂ ), tungsten oxide (WO ₂ , WO ₃ ).

Examples of the nitride of the element constituting the first metal include calcium nitride (Ca ₃ N ₂ ), strontium nitride (Sr ₃ N ₂ ), barium nitride (Ba ₃ N ₂ ), scandium nitride (ScN), and yttrium nitride. (YN), lanthanum nitride (LaN), cerium nitride (CeN), praseodymium nitride (PrN), neodymium nitride (NdN), titanium nitride (TiN), zirconium nitride (ZrN), hafnium nitride (HfN), vanadium nitride (VN) ), Niobium nitride (NbN), tantalum nitride (TaN), chromium nitride (Cr ₂ N, CrN), molybdenum nitride (Mo ₂ N, MoN), tungsten nitride (W ₂ N, WN ₂ , W ₂ N ₃ ), Titanium zirconium nitride (TiZrN), titanium hafnium nitride (TiHfN), titanium vanadium nitride TiVN), titanium niobium nitride (TiNbN), titanium tantalum nitride (TiTaN), titanium chromium chromium (TiCrN), titanium molybdenum nitride (TiMoN), titanium tungsten nitride (TiWN), zirconium nitride hafnium (ZrHfN), zirconium vanadium nitride (ZrVN) , Zirconium niobium nitride (ZrNbN), zirconium tantalum nitride (ZrTaN), zirconium nitride chromium (ZrCrN), zirconium molybdenum molybdenum (ZrMoN), zirconium tungsten nitride (ZrWN), hafnium vanadium nitride (HfVN), hafnium niobium nitride (HfNbN), Hafnium tantalum nitride (HfTaN), hafnium chrome nitride (HfCrN), hafnium molybdenum nitride (HfMoN), hafnium nitride Tungsten (HfWN), vanadium niobium nitride (VNbN), vanadium tantalum nitride (VTaN), vanadium chromium nitride (VCrN), vanadium nitride molybdenum (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 molybdenum nitride (TaMoN), tantalum tungsten nitride (TaWN), chromium molybdenum nitride (CrMoN), chromium tungsten nitride (CrWN) ), Molybdenum nitride chromium (MoWN).

  Examples of the oxynitride of the element constituting the first metal include titanium oxynitride (TiON), zirconium oxynitride (ZrON), hafnium oxynitride (HfON), vanadium oxynitride (VON), and niobium oxynitride (NbON). Tantalum oxynitride (TaON), chromium oxynitride (CrON), molybdenum oxynitride (MoON), tungsten oxynitride (WON), silicon oxynitride (SiON), and boron oxynitride (BON).

Examples of the silicon-containing particles include silicon particles made of only silicon and silicon compound particles such as silicon nitride (Si ₃ N ₄ ), silicon oxide (SiO ₂ ), and silicon oxynitride (SiON).

Examples of the particles containing aluminum include aluminum particles made of only aluminum, aluminum nitride (AlN), aluminum oxide (Al ₂ O ₃ ), aluminum oxynitride (AlON), YAG (Y ₃ Al ₅ O ₁₂ ), and the like. The particle | grains of an aluminum compound are mentioned.

  Alternatively, particles containing silicon and aluminum at the same time may be used. An example is sialon particles (SiAlON).

  The first metal-containing particles, silicon-containing particles, and aluminum-containing particles are weighed so that the ratio of the first metal, silicon, and aluminum is a desired ratio, and then these particles are mixed by a ball mill or a jet mill. . The average particle size of the particles contained in the first particle group after mixing is preferably 10 μm or less. When the first particle group having such an average particle size is used, the application of nitrogen and oxygen to the first particle group can be made more uniform in the second particle group production step described later, and thus the intended composition The second particle group can be produced with high yield. In the present specification, the average particle diameter of the particles means a median diameter based on the particle size distribution of the particles measured by a known particle size distribution measuring method such as a laser diffraction method.

  The obtained first particle group is preferably pressure-molded for use in the second particle group preparation step described later. The method of pressure molding is not particularly limited, and a known method can be used. For example, the first particle group can be pressurized to 1 MPa or more and 150 MPa or less to obtain a pressure molded body.

(Second particle group production process)
Next, referring to FIG. 1, in the second particle group production step (S2), the first particle group is heat-treated to produce a second particle group containing the first metal, silicon, aluminum, oxygen and nitrogen. To do. By the heat treatment, one or both of a shortage of nitrogen and oxygen are imparted to the first particle group, and the second particle group having the same composition ratio as the target cubic sialon can be obtained. The “shortage of nitrogen and oxygen” corresponds to the difference between the content ratio of nitrogen and oxygen in the first particle group and the content ratio of nitrogen and oxygen in the target cubic sialon.

  For the heat treatment, a method of applying heat to the first particle group from the outside (hereinafter also referred to as an external heating method) or a method using a reaction by self-heating of the first particle group (hereinafter also referred to as a combustion synthesis method) is used. Can do.

  In the external heating method, for example, a powder composed of the first particle group or a molded body formed by pressure-molding the first particle group is subjected to a vacuum atmosphere or from argon gas, nitrogen gas and oxygen gas. It arrange | positions in the atmosphere containing 1 or more types of gas selected from the group which consists of, and heats from the outside using a carbon heater etc. The atmosphere in which the first particle group is placed is appropriately selected depending on the composition of the first particle group.

  For example, when the first particle group is composed of each element of the first metal, silicon, and aluminum and does not contain any element of nitrogen and oxygen, the first particle group is placed in an atmosphere containing nitrogen gas and oxygen gas. Will be. This is because the total amount of both nitrogen and oxygen in the target cubic sialon needs to be applied from the source gas used in the external heating method. Further, for example, when the first particle group contains the first metal, aluminum, silicon and nitrogen at the same ratio as the target cubic sialon and does not contain oxygen, the first particle group contains nitrogen gas. It does not contain, but is placed in an atmosphere containing oxygen gas. For example, when the first particle group includes the first metal, aluminum, silicon, nitrogen, and oxygen at the same ratio as the target cubic sialon, the first particle group is an atmosphere composed of only argon gas. It can be placed under or under a vacuum atmosphere.

  By appropriately adjusting the heating temperature of the atmosphere in which the first particle group is placed and the partial pressure of each gas, the amount of oxygen applied to the first particle group and the amount of nitrogen can be controlled. Further, the amount of oxygen and the amount of nitrogen imparted to the first particle group can also be controlled by the processing time of the heating step.

  The heating temperature, the partial pressure of each gas, and the heating time in the external heating method are appropriately adjusted. For example, the heating temperature is preferably 1500 ° C. or higher and 2000 ° C. or lower, more preferably 1700 ° C. or higher and 1900 ° C. or lower. The partial pressure of each gas is preferably 0.1 MPa or more, and more preferably 0.3 MPa or more. The heating time is preferably 6 hours or more.

  The combustion synthesis method is a powder synthesis method that utilizes high heat of chemical reaction that is released when a target compound is synthesized. According to the combustion synthesis method, the target compound can be obtained in a short time in units of seconds. The combustion synthesis method does not require external energy supply, and has advantages such as reduction in synthesis cost.

  In the combustion synthesis method, for example, a compact obtained by pressure-molding the first particle group is charged into a furnace, and the furnace is filled with a nitrogen gas atmosphere. Next, after setting the partial pressure of nitrogen gas in the furnace to 1 MPa or more and 15 MPa or less, the end portion of the compact is heated to induce the nitriding reaction of the first particle group. The chemical reaction heat generated by the nitriding reaction induces the reaction of the adjacent portion, so that the chemical reaction propagates to the entire molded body, and the second particle group can be obtained.

  The amount of nitrogen applied to the first particle group can be controlled by appropriately adjusting the partial pressure of the atmospheric gas in the furnace in which the first particle group is placed. Further, the amount of nitrogen applied to the first particle group can also be controlled by the processing time of the heating step.

When the combustion synthesis method is used, the first particle group needs to contain 20% by weight or more of a nitridable component. Here, the nitridable component means particles composed of one kind of metal element constituting the first metal, particles composed of an alloy containing two or more kinds of metal elements constituting the first metal, and nitriding with an insufficient amount of nitrogen. Means (for example, Ti ₂ N, Ca ₂ N, etc.) and the like.

  The obtained second particle group is preferably pulverized for use in a cubic sialon manufacturing process described later. The method for pulverization is not particularly limited, and a known method can be used. For example, the second particle group is roughly crushed using a cemented carbide rod, passed through a 150 μm mesh, and then finely ground using a ball mill or a jet mill. The average particle size of the second particle group is preferably from 0.1 μm to 10 μm, and more preferably from 0.5 μm to 3 μm.

(Cubic sialon manufacturing process)
Next, referring to FIG. 1, in the cubic sialon production step (S3), the second particle group is processed by an impact compression method or a static pressure synthesis method to produce a cubic sialon.

  In the impact compression method, for example, the second particle group is mixed with a heat sink and copper powder as a pressure medium, 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. By applying pressure, the second particle group can be converted into cubic sialon. The pressure for impact pressing is preferably 15 GPa or more and 50 GPa or less, and more preferably 20 GPa or more. The pressing time at the time of impact pressing is preferably 1 microsecond or more and 50 microsecond or less, and more preferably 3 microsecond or more and 40 microsecond or less. The temperature at the time of impact pressing is preferably 1200 ° C. or higher and 3000 ° C. or lower, more preferably 1500 ° C. or higher and 2500 ° C. or lower.

  In the static pressure synthesis method, for example, the second particle group is treated using a multi-anvil press or the like under conditions of a pressure of 0.1 GPa to 20 PGa and a temperature of 1000 ° C. to 2000 ° C. for 5 minutes to 180 minutes. The second particle group can be converted into cubic sialon.

  When the second particle group is processed by the impact compression method or the hydrostatic synthesis method, a part of the second particle group becomes an inevitable impurity without being converted into cubic sialon. Inevitable impurities include, for example, oxides, nitrides, oxynitrides, silicon nitrides, silicon oxides, aluminum oxides of elements selected from the group consisting of Group 4 elements, Group 5 elements and Group 6 elements of the Periodic Table , Aluminum nitride, tungsten carbide, and amorphous materials. The total amount of these inevitable impurities is preferably 10% by mass or less, more preferably 5.0% by mass or less, in a total of 100% by mass of cubic sialon and inevitable impurities.

  In order to remove inevitable impurities, it is preferable to purify cubic sialon from the powder after the treatment by the impact compression method or the static pressure synthesis method.

  The purification of the cubic sialon can be performed, for example, by the following method. First, the powder after the treatment by the impact compression method or the static pressure synthesis method is finely pulverized using a ball mill or a jet mill. The obtained pulverized powder is washed with an acidic solution such as hydrofluoric acid. Since the amorphous substance is dissolved in the acidic solution, the amorphous substance can be removed by washing the powder with the acidic solution. Next, the purified cubic sialon can be obtained by separating the cubic sialon and the inevitable impurities contained in the washed powder using centrifugation or the like.

<Fifth Embodiment>
The manufacturing method of the sintered compact concerning 5th Embodiment is demonstrated using FIG.

The method for producing a sintered body comprises a group consisting of calcium, strontium, barium, scandium, yttrium, lanthanoid, manganese, iron, cobalt, nickel, copper, Group 4 element, Group 5 element and Group 6 element of the periodic table A step of preparing a first particle group including at least one first metal selected from the group consisting of silicon and aluminum (shown as S21 in FIG. 2; hereinafter, also referred to as “first particle group preparation step”); The step of heat-treating the first particle group to produce a second particle group containing the first metal, silicon, aluminum, oxygen and nitrogen (shown as S22 in FIG. 2). (Also referred to as a “step”), the second particle group is treated by an impact compression method or a static pressure synthesis method to produce a cubic sialon (shown as S23 in FIG. 2). And a step of preparing a third particle group containing 20% by volume or more and 100% by volume or less of cubic sialon (referred to as S24 in FIG. 2). And a step of producing a sintered body by sintering the third particle group (indicated as S25 in FIG. 2) (also referred to as a “sintered body producing step”). The cubic sialon has the following formula (1)
M _x Si _(6-xy) Al _y O _y N _(8-y) (1)
(In the formula (1), M is composed of calcium, strontium, barium, scandium, yttrium, lanthanoid, manganese, iron, cobalt, nickel, copper, Group 4 element, Group 5 element and Group 6 element of the periodic table. A first metal including at least one selected from the group, and satisfying the relationship of 0.01 ≦ y ≦ 4.2 and 1.79 ≦ (6-xy) ≦ 5.98).

  The first particle group production step (S21), the second particle group production step (S22), and the cubic sialon production step (S23) are respectively the first particle group production step (S1) and the second of the fourth embodiment. Since it is similar to the particle group production step (S2) and the cubic sialon production step (S3), the description thereof will not be repeated.

(Third particle group preparation step)
Referring to FIG. 2, in the third particle group preparation step (S24), a third particle group containing 20% by volume or more and 100% by volume or less of the cubic sialon prepared in the cubic sialon manufacturing step (S23) is prepared. .

  A 3rd particle group is a raw material particle group used as the raw material of a sintered compact. The third particle group may contain only cubic sialon, or may contain a material that becomes a raw material of the binder phase together with cubic sialon.

  For example, the second metal and the first compound described in the second embodiment can be used as the material for the binder phase. Note that the second metal and the first compound are the same as those in the second embodiment, and thus description thereof will not be repeated.

  The content of cubic sialon in the third particle group is 20% by volume or more and 100% by volume or less. When the content of the cubic sialon in the third particle group is 20% by volume or more, the wear resistance and fracture resistance of the sintered body obtained by sintering the third particle group are improved. The content of cubic sialon in the third particle group is preferably 50% by volume to 100% by volume, more preferably 50% by volume to 90% by volume, and further preferably 50% by volume to 80% by volume.

  When the third particle group includes a cubic phase sialon and a binder phase raw material, it is preferable to mix the third particle group using a ball mill or a jet mill.

(Sintered body production process)
Next, referring to FIG. 2, in the sintered body manufacturing step (S25), the third particle group is sintered to prepare a sintered body.

  The sintering of the third particle group is preferably performed after the third particle group is pressure-molded. Moreover, you may carry out simultaneously with pressure molding. Examples of methods for simultaneously performing pressure molding and sintering include a hot press (HP) method, a discharge plasma sintering (SPS) method, and an ultra-high pressure sintering method. Moreover, after shaping | molding by the cold isostatic pressing (CIP) method, it can also sinter using a hot isostatic pressing (HIP) method. In addition, you may use a normal pressure sintering method instead of the above pressure sintering methods.

  The sintered body preparation step is preferably performed in a non-oxidizing and non-nitriding atmosphere in order to prevent the composition of the sintered body from greatly changing from the composition of the third particle group.

  The pressure during sintering is preferably 0.1 GPa or more and 20 GPa or less, and more preferably 1 GPa or more. The temperature during sintering is preferably 1000 ° C. or higher and 2000 ° C. or lower, more preferably 1300 ° C. or higher and 1700 ° C. or lower. The time required for sintering varies depending on the amount (volume) of the third particle group, the temperature, and the like. For example, when the sintering temperature is 1000 ° C. or more and 2000 ° C. or less, it can be 3 minutes or more and 180 minutes or less. .

  By performing the sintered body manufacturing step, a sintered body containing a cubic sialon represented by the above formula (1) can be obtained.

  The present invention will be described more specifically with reference to examples. However, the present invention is not limited to these examples.

[Sample 1-1 to Sample 1-50, 1-52, 1-53]
<Production of cubic sialon>
(First particle group preparation step)
According to the raw materials and mixing ratios in Table 1, a first particle group in which raw material particles were mixed was prepared. For example, in Sample 1-1, after measuring Si ₃ N ₄ particles, Al ₂ O ₃ particles, and TiO ₂ particles so that the mixing ratio (mass ratio) is 67:18:15, the ball mill To prepare a first particle group. The average particle diameters of the first particle groups prepared in Sample 1-1 to Sample 1-50, 1-52, 1-53 were all 10 μm or less. The obtained first particle group was pressure-molded at a pressure of 10 MPa to obtain a molded body.

(Second particle group production process)
Next, the compact | molding | casting of the 1st particle group was heat-processed, and the 2nd particle group was produced. Table 1 shows the heat treatment method used for each sample. In Table 1, “external heating” means an external heating method, and “combustion synthesis” means a combustion synthesis method.

  In the external heating method, first, the first particle group was placed in a crucible filled with nitrogen gas. And the inside of a crucible was heated at 1700 degreeC with the carbon heater arrange | positioned around the crucible. At this time, the gas pressure in the crucible was 0.3 MPa. The heating time after the inside of the crucible reached 1700 ° C. was 6 hours. Thereby, the 2nd particle group was obtained.

  In the combustion synthesis method, first, the first particle group was disposed in a pressure vessel having a gas supply unit and a gas discharge unit. Then, nitrogen gas is supplied into the pressure vessel, the pressure is increased to 3 MPa, and a part of the first particle group is ignited using a heat source of 1500 ° C. The combustion time after igniting a part was 1 minute. Thereby, the 2nd particle group was obtained.

  The obtained second particle group was roughly hit using a cemented carbide rod, passed through a 150 μm mesh, and then pulverized using a ball mill. The average particle size of the second particle group after pulverization was 1 μm.

(Cubic sialon manufacturing process)
Next, the obtained 2nd particle group was processed by the impact compression method or the static pressure synthesis method, and the cubic sialon was produced. Table 1 shows the synthesis method used for each sample. In Table 1, “impact compression” means the impact compression method, and “static pressure synthesis” means the static pressure synthesis method.

  In the impact compression method, first, the second particle group was mixed with a heat sink and copper powder and filled into a steel container. Thereafter, the second particle group was treated for 5 microseconds at a pressure of 15 GPa and a temperature of 2000 ° C. by explosion of an explosive to obtain a sample containing cubic sialon.

In the static pressure synthesis method, the second particle group was treated with a cemented carbide anvil at a pressure of 15 GPa and a temperature of 2000 ° C. for 15 minutes to obtain a sample containing cubic sialon.
.

  The obtained sample containing cubic sialon was pulverized with a ball mill. The ground sample was treated with nitric acid to remove impurities. Further, the cubic sialon was purified by centrifugation and classified with a water tank.

<Measurement of cubic sialon>
The resulting cubic sialon was subjected to X-ray diffraction measurement to identify the product phase. The results are shown in the “Product” column of Table 1.

Furthermore, high frequency inductively coupled plasma optical emission spectrometry was performed to examine the proportion of metal elements in cubic sialon. Further, the ratio of oxygen element and nitrogen element in the cubic sialon was examined by an inert gas melting infrared absorption method. Also it performs processing to allow the obtained powder of the cross-section is observed, scanning (hereinafter referred to as SEM) electron microscopy of the powder of the cross section was observed, in color density in the powder, that have a solid solution of a metal element and support Iaron particles, to distinguish the metal element dispersed in the sialon particles inside and outside. At that time, each compound was characterized by elemental analysis in advance. Furthermore, the visual field was binarized to quantify the amount of dispersed metal elements. From these results, the values of x, y and dispersed metal components in the above formula (1) indicating cubic sialon were calculated. The results are shown in the “x” and “y” columns of Table 1 . Name your, it was described in the column of the product of Table 1 as "c-" means "cubic".

<Preparation of sintered body>
The obtained cubic sialon was sintered at the pressure, temperature and sintering time shown in Table 1 to obtain a sintered body. EPMA (Electron Probe X-ray Micro Analyzer: attached to the scanning electron microscope: characteristic X-rays generated when the sample is irradiated with an electron beam for each of the cubic sialon before sintering and the obtained sintered body As a result of the analysis by a device for detecting the constituent elements and analyzing the constituent elements, both have the same constituent element ratio. That is, it was confirmed that the cubic sialon hardly changes in constituent element ratio before and after sintering.

<Evaluation of sintered body>
The obtained sintered body was processed using a laser to prepare a chamfer-shaped cutting tool having a chip shape of ISO model number CNGA120408, a cutting edge treatment of −25 °, and a width of 0.15 mm. A cutting test was performed under the following cutting conditions, and the cutting length (km) until the average flank wear amount during continuous cutting reached 200 μm and the cutting length (km) until the chipping during intermittent cutting were measured.

(Continuous cutting conditions and evaluation details)
Work Material: Outer Diameter Machining of Inconel 718 (Registered Trademark) Round Bar Work Material Hardness: HRC40
Cutting speed: V = 150 m / min
Cutting depth: d = 0.25 m / min
Feeding speed: f = 0.1mm / rev
Coolant: Emulsion diluted 20 times Details of evaluation: Cutting length (km) until average flank wear reaches 200 μm
(Intermittent cutting conditions and evaluation details)
Work Material: Outside Diameter Processing of Inconel 718 (Registered Trademark) Bar with Grooves at Four Peripheries Work Material Hardness: HRC40
Cutting speed: V = 150 m / min
Cutting depth: d = 0.25 m / min
Feeding speed: f = 0.1mm / rev
Coolant: None Content of evaluation: Cutting length to the defect (km)
The results are shown in Table 1. The longer the cutting length (km) until the average flank wear amount during continuous cutting reaches 200 μm, the better the wear resistance. The longer the cutting length (km) to the fracture during intermittent cutting, the better the fracture resistance.

[Sample 1-51]
In Sample 1-51, a sintered body was produced using conventional cubic sialon (Si _(6-x) Al _x O _x N _(8-x) (0 <x ≦ 4.2)). A cutting tool having the same shape as that of Sample 1-1 was produced using the obtained sintered body, and the same evaluation as that of Sample 1-1 was performed. The results are shown in Table 1.

<Evaluation results>
The sintered bodies of Sample 1-1 to Sample 1-50 are sintered bodies manufactured using cubic sialon represented by the above formula (1). Abrasion resistance and fracture resistance were superior to the sintered body of Sample 1-51 produced using conventional cubic sialon.

[Sample 2-1 to Sample 2-35, Sample 2-39, Sample 2-40]
<Preparation of sintered body>
Sample 1-1, Sample 1-15, Sample 1-29 or Sample 1-38 cubic sialon and the second metal or first compound are mixed in the ratio shown in Table 2 to produce the third particle group. did. The third particle group was sintered by the HP method at the pressure, temperature and sintering time shown in Table 2 to obtain a sintered body. As a result of X-ray diffraction of the obtained sintered body, it was confirmed that the mass ratio of cubic sialon in the third particle group and the mass ratio of cubic sialon in the sintered body hardly changed. . In addition, each of the third particle group and the obtained sintered body is detected with EPMA (Electron Probe X-ray Micro Analyzer: attached to the scanning electron microscope). As a result of analysis using a device for analyzing constituent elements, both constituent elements have similar constituent element ratios. That is, it was confirmed that the constituent element ratio hardly changed between the third particle group and the sintered body.

<Evaluation of sintered body>
Using the obtained sintered body, a cutting tool having the same shape as that of Sample 1-1 was produced, and the same evaluation as that of Sample 1-1 was performed. The results are shown in Table 2.

[Sample 2-36 to Sample 2-38]
In Sample 2-36, a sintered body was manufactured using conventional cubic sialon (Si _(6-x) Al _x O _x N _(8-x) (0 <x ≦ 4.2)).

In Sample 2-37, a sintered body was formed using a conventional cubic sialon (Si _(6-x) Al _x O _x N _(8-x) (0 <x ≦ 4.2)) and β-sialon. Produced.

In Sample 2-38, a sintered body was produced using conventional cubic sialon (Si _(6-x) Al _x O _x N _(8-x) (0 <x ≦ 4.2)) and cobalt. .

<Evaluation of sintered body>
Using the obtained sintered body, a cutting tool having the same shape as that of Sample 1-1 was produced, and the same evaluation as that of Sample 1-1 was performed. The results are shown in Table 2.

<Evaluation results>
The sintered bodies of Sample 2-1 to Sample 2-35 are sintered bodies produced using the cubic sialon represented by the above formula (1), and contain cubic sialon in the sintered body. The amount is 20% by volume or more and 80% by volume or less.

  The sintered bodies of Sample 2-36 to Sample 2-38 are sintered bodies manufactured using conventional cubic sialon.

  The sintered bodies of Samples 2-39 to 2-40 are sintered bodies produced using the cubic sialon represented by the above formula (1), and contain cubic sialon in the sintered body. The amount is 15% by volume.

  The sintered bodies of Sample 2-1 to Sample 2-35 were superior in wear resistance and fracture resistance as compared to the sintered bodies of Sample 2-36 to Sample 2-40.

  The embodiments and examples disclosed herein are illustrative in all respects and should not be construed as being restrictive. The scope of the present invention is shown not by the above-described embodiment but by the scope of claims, and is intended to include meanings equivalent to the scope of claims and all modifications within the scope.

  The sintered body containing cubic sialon according to an embodiment of the present invention can be widely used for cutting tools. For example, 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.

Claims (7)

Following formula (1)
M _x Si _(6-xy) Al _y O _y N _(8-y) (1)
In (formula (1), M comprises calcium, strontium, barium, scandium, yttrium, lanthanides, Group IV of the periodic table, at least one selected from the group consisting of group 5 element and a group 6 element (It is a first metal and satisfies the relationship of 0.01 ≦ x ≦ 1.5 , 0.01 ≦ y ≦ 4.2, and 1.79 ≦ (6-xy) ≦ 5.98)
Cubic sialon represented by The sintered compact containing 20 volume% or more and 100 volume% or less of the cubic sialon of Claim 1 . A sintered body comprising the cubic sialon according to claim 1 and any one or both of a second metal and a first compound,
The second metal includes at least one selected from the group consisting of manganese, iron, cobalt, nickel and copper,
The first compound is at least selected from the group consisting of aluminum, boron, silicon, manganese, iron, cobalt, nickel, copper, calcium, yttrium, Group 4 element, Group 5 element and Group 6 element of the Periodic Table The sintered body according to claim 3, comprising at least one compound composed of one kind of first element and at least one kind of second element selected from the group consisting of carbon, nitrogen, oxygen and boron. Cutting tool comprising a sintered body according to claim 2 or claim 3. A method for producing a cubic sialon according to claim 1,
Calcium, strontium, barium, scandium, yttrium, lanthanides, Group IV of the periodic table, the first metal comprising at least one selected from the group consisting of group 5 element and a group 6 element, silicon, and aluminum Preparing a first particle group comprising:
Heat-treating the first particle group to produce a second particle group containing the first metal, silicon, aluminum, oxygen and nitrogen;
Said second particle group by treatment with shock compression method or static synthesis, Ru and a step of preparing a cubic sialon, cubic method for producing sialon. It is a manufacturing method of the sintered compact according to claim 2 or 3,
Calcium, strontium, barium, scandium, yttrium, lanthanides, Group IV of the periodic table, the first metal comprising at least one selected from the group consisting of group 5 element and a group 6 element, silicon and aluminum Preparing a first particle group;
Heat-treating the first particle group to produce a second particle group containing the first metal, silicon, aluminum, oxygen and nitrogen;
Treating the second particle group by impact compression or static pressure synthesis to produce cubic sialon;
Preparing a third particle group containing 20% by volume or more and 100% by volume or less of the cubic sialon;
Ru and a step of obtaining a sintered body by sintering said third particle group, the production method of the sintered body. The third particle group includes the cubic sialon, and one or both of the second metal and the first compound,
The second metal includes at least one selected from the group consisting of manganese, iron, cobalt, nickel and copper,
The first compound is at least selected from the group consisting of aluminum, boron, silicon, manganese, iron, cobalt, nickel, copper, calcium, yttrium, Group 4 element, Group 5 element and Group 6 element of the Periodic Table The production of a sintered body according to claim 6 , comprising at least one compound composed of one kind of first element and at least one kind of second element selected from the group consisting of carbon, nitrogen, oxygen and boron. Method.

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