WO2016076656A1 - Ceramic material and cutting tools made thereof - Google Patents

Ceramic material and cutting tools made thereof Download PDF

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WO2016076656A1
WO2016076656A1 PCT/KR2015/012203 KR2015012203W WO2016076656A1 WO 2016076656 A1 WO2016076656 A1 WO 2016076656A1 KR 2015012203 W KR2015012203 W KR 2015012203W WO 2016076656 A1 WO2016076656 A1 WO 2016076656A1
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polytype
ceramic material
sialon
phase
ratio
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Sung Su Chun
Dae Yeop Lee
Geun Ho Park
Chang Hoon HONG
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Taegutec Ltd
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Taegutec Ltd
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Priority to EP15859663.5A priority Critical patent/EP3218323B1/en
Priority to JP2017522517A priority patent/JP2018500259A/en
Priority to US15/522,007 priority patent/US10000420B2/en
Publication of WO2016076656A1 publication Critical patent/WO2016076656A1/en
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/597—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon oxynitride, e.g. SIALONS
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23B—TURNING; BORING
    • B23B27/00—Tools for turning or boring machines; Tools of a similar kind in general; Accessories therefor
    • B23B27/14—Cutting tools of which the bits or tips or cutting inserts are of special material
    • B23B27/148—Composition of the cutting inserts
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
    • C01B21/0821—Oxynitrides of metals, boron or silicon
    • C01B21/0826—Silicon aluminium oxynitrides, i.e. sialons
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    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
    • C04B35/62655—Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • C04B35/645—Pressure sintering
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23B—TURNING; BORING
    • B23B2222/00—Materials of tools or workpieces composed of metals, alloys or metal matrices
    • B23B2222/64—Nickel
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23B—TURNING; BORING
    • B23B2226/00—Materials of tools or workpieces not comprising a metal
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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    • C04B2235/74—Physical characteristics
    • C04B2235/76—Crystal structural characteristics, e.g. symmetry
    • C04B2235/767—Hexagonal symmetry, e.g. beta-Si3N4, beta-Sialon, alpha-SiC or hexa-ferrites
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Definitions

  • the present disclosure relates to a silicon nitride ceramic material having wear resistance and toughness suitable for machining heat resistant super alloy (HRSA), and a cutting tool made of the same.
  • HRSA heat resistant super alloy
  • the high hot hardness of a ceramic material allows the ceramic material for cutting tools to be an appropriate choice for machining a workpiece which has high hardness, high tensile strength and low thermal expansion at elevated temperature, and it is particularly suitable for a self-hardening material such as nickel- or cobalt-based material which is often used for the heat resistant super alloy (HRSA).
  • HRSA heat resistant super alloy
  • nitride silicon materials for cutting tools are fabricated using aluminum oxide Al 2 O 3 as a sintering additive. Because aluminum and oxygen can replace the silicon and nitrogen in silicon nitride crystal structure respectively, these can form so-called "sialon" ceramic.
  • the sialon ceramic consists of silicon, aluminum, oxygen and nitrogen (Si-Al-O-N) and can sometimes be additionally stabilized by cation (Me), in which Me n+ may refer to a material having proper ion radius (r ⁇ 1.0 ⁇ ) with a plurality of rare earth metals, and may be selected from lanthanide such as Y, Yb, Dy, Lu, Li, Ca, Mg, Sc, for example.
  • the main phase for use in cutting tools remains in ⁇ -sialon phase, i.e., in R x Si 12 - (m+n) Al (m+n) O n N (16-n) (1.0 ⁇ m ⁇ 2.7; n ⁇ 1.2) state, in which R is one of the above-mentioned metals or the lantanoide having smaller ion radius than 1.0 ⁇ , and ⁇ -sialon is Si 6 - z Al z O z N (8-z) (0 ⁇ z ⁇ 4.2).
  • the materials such as silicon nitride, alumina, AlN or a number of materials such as 12H, 21R used as a sialon polyphase (or polytype) composition temporarily form a molten material with lanthanoid or metal, or with lantanoid oxide.
  • ⁇ - and ⁇ -sialon phases if Y is used as metal ion R described above
  • different phases such as YAG, melilite, B-phase, 12H and so on are crystallized.
  • the intergranular phase among crystalline particles remains. The amount of the produced intergranular phase is influenced by the composition of the materials and sintering conditions used.
  • the metal ion can not only act to stabilize the ⁇ -sialon phase, but also act as a catalyst to form sialon crystals during sintering. It usually aids forming of elongated sialon particles in ⁇ -phase, but elongated ⁇ -sialon particles are also produced. (Refer to "Nucleation and Growth of the Elongated ⁇ -SiAlON" by Fang-Fang X, Shu-Lin W, Nordberg L O, Ekstrom T (J. Eur. Ceram. Soc. 17(13) 1631-1638 (1997)).
  • US 7,629,281 proposes a ceramic material comprising ⁇ -sialon, 12H, and intergranular amorphous or partly crystalline phase and yittrium.
  • An object of the present disclosure is to provide a silicon nitride ceramic material for a metal cutting tool, having wear resistance and toughness suitable for machining heat resistant super alloy (HRSA).
  • HRSA heat resistant super alloy
  • An object of the present disclosure is to provide a cutting tool made of a silicon nitr ⁇ ide ceramic material for a metal cutting tool, which has wear resistance and toughness for machining heat resistant super alloy (HRSA).
  • HRSA heat resistant super alloy
  • a ceramic material consists of ⁇ -sialon (Si (6-z) Al z O z N (8-z) ) and polytype 15R and intergranular phase, and contains yittrium, in which the polytype 15R includes twin grains.
  • the amount of the polytype 15R is between 25% and 55%, as measured as a ratio of the height in a Cu-K ⁇ X-ray diffraction pattern of 15R peak at a 2 ⁇ value of 34° and the height in the same diffraction pattern of the ⁇ -sialon peak at a 2 ⁇ value of 33°.
  • a ceramic material which has wear resistance and toughness proper for use in a cutting tool to machine heat resistant super alloy (HRSA).
  • HRSA machine heat resistant super alloy
  • FIG. 1 shows an X-ray diffraction pattern from a ceramic material according to an exemplary embodiment
  • FIG. 2 is a Scanning Electron Microscope (SEM) micrograph of a ceramic material according to an exemplary embodiment
  • FIG. 3 shows a variation of Vickers hardness (H V ) according to ratio of polytype 15R;
  • FIG. 4 shows a variation of Rockwell hardness (H Ra ) according to ratio of polytype 15R;
  • FIG. 5 shows a variation of fracture toughness (K IC ) according to ratio of polytype 15R;
  • FIG. 6 shows a variation of brittleness (B I ) according to ratio of polytype 15R;
  • FIG. 7 shows a variation of wear resistance (R W ) according to ratio of polytype 15R.
  • FIG. 8 shows a milling test result of a cutting tool according to an exemplary embodiment.
  • Y 2 O 3 content and MgO content which include metal ions for use as a catalyst in the preparation of the ceramic material, are fixed at 4 wt%.
  • Powder mixture mixed at wt% according to [Table 1] is added with methanol as a solvent, a dispersant and a binder, and milled with a ball mill for about 20 hr.
  • the raw materials are milled as described above so that a slurry of the raw materials is prepared.
  • the slurry After milling to prepare slurry, the slurry is granulated through a spray dryer. Powder is obtained by passing the granulated raw materials through a sieve.
  • the obtained powder is compressed into a compact.
  • the compact is subject to de-binding, and then sintered and densified during 2 hours of gas pressure sintering at 1680°C ⁇ 1820°C.
  • [Table 2] below shows the ceramic material prepared from the Examples shown in [Table 1] by the procedures described above. Further, the prepared ceramic material was analyzed with the X-ray diffractography.
  • FIG. 1 shows an X-ray diffraction pattern from a ceramic material according to an exemplary embodiment.
  • ⁇ represents ⁇ -sialon (Si 6 - z Al z O z N (8-z) ), and 15R represents polytype 15R phase.
  • FIG. 1 shows the X-ray diffraction pattern of Example 14 (No. 14) for an example.
  • the ceramic material according to an exemplary embodiment includes ⁇ -sialon, but does not include ⁇ -sialon. Further, based on the peak around 34° and a plurality of satellite peaks shown in FIG. 1, it is understood that the ceramic material according to an exemplary embodiment includes the polytype 15R phase.
  • a z value of the ⁇ -sialon included in the ceramic material prepared according to Examples of the present disclosure can be determined.
  • the amount of the polytype 15R phase can be determined based on the ratio of the height in a Cu-K ⁇ X-ray diffraction pattern of 15R peak at a 2 ⁇ value (b) of 34°, and the ratio of the height in a Cu-K ⁇ X-ray diffraction pattern of the ⁇ -sialon peak at a 2 ⁇ value (a) of 33°.
  • FIG. 2 is a Scanning Electron Microscope (SEM) micrograph of a ceramic material according to an exemplary embodiment.
  • FIG. 2 is the SEM micrograph of a sample prepared from Example 14 (No. 14).
  • the ceramic material consists of ⁇ -sialon, polytype 15R phase, and intergranular phase between ⁇ -sialon and polytype 15R phase.
  • the polytype 15R phase includes crystal grains of bright bands and dark bands repeatedly stacked on one another. Such crystal grains may be the twin grains. Accordingly, it is understood that, in the ceramic material according to an exemplary embodiment, the polytype 15R phase may include twin grains.
  • Example 2 and Example 10 that include MgO do not form polytype 15R phase.
  • the Examples that form the polytype 15R phase use Y 2 O 3 as a catalyst.
  • the ceramic material according to an exemplary embodiment may consist of ⁇ -sialon, polytype 15R phase and intergranular phase between ⁇ -sialon and polytype 15R phase, and may contain yittrium (Y) which was included in the raw material.
  • the polytype 15R phase may include twin grains.
  • Examples 1 to 16 were tested for Vickers hardness (H V ), Rockwell hardness (H Ra ) and fracture toughness (K IC ), as shown in [Table 3] below.
  • H V Vickers hardness
  • H Ra Rockwell hardness
  • K IC fracture toughness
  • the Vickers hardness (H V ) was measured, by pressing with a square base diamond pyramid indenter consisting of a 136 degree included angle between opposite faces under 10kg load, and measuring a diagonal line of the concave portion. At this time, the descending speed of the indenter was 150 ⁇ m/s, and 15 seconds of indentation time was maintained.
  • H Ra Rockwell hardness
  • a steel ball of a predetermined shape or a diamond cone-shaped indenter was used to exert an initial reference load, after which the load was increased to test load (60 kgf in the measuring of the present disclosure). The load was then returned to the initial reference load.
  • the Rockwell hardness was then defined based on the difference of depths of the two indentations, i.e., the difference between the depth under reference loading and depth of the indentation.
  • FIG. 3 shows a variation of Vickers hardness (H V ) according to ratio of polytype 15R.
  • FIG. 4 shows a variation of Rockwell hardness (H Ra ) according to ratio of polytype 15R.
  • FIG. 5 shows a variation of fracture toughness (K IC ) according to ratio of polytype 15R.
  • the Vickers hardness (H V ) or the Rockwell hardness (H Ra ) shows decreasing tendency as the ratio of polytype 15R increases.
  • [Table 4] shows the brittleness index (B I ) and wear resistance (R W ) according to different ratios of polytype 15R.
  • the brittleness index (B I ) is proportional to the Vickers hardness (H V ), but is inversely proportional to the fracture toughness (K IC ). [Mathematical equation 2] as below is used to obtain the brittleness index (B I ) in [Table 4].
  • the wear resistance (R W ) in [Table 4] is an index to the frictional wear excluding chemical wear, which is inversely proportional to the Vickers hardness (H V ), but is proportional to the fracture toughness (K IC ). Also notable is higher sensitivity to the variation of fracture toughness (K IC ), than to the Vickers hardness (H V ). [Mathematical equation 3] as below is used to obtain the wear resistance (R W ) in [Table 4].
  • FIG. 6 shows a variation of brittleness (B I ) according to ratio of polytype 15R.
  • FIG. 7 shows a variation of wear resistance (R W ) according to ratio of polytype 15R.
  • a ceramic material having between 25% and 55% of a ratio of polytype 15R phase may have lower brittleness index, but have higher wear resistance than the ceramic materials including polytype 15R phase of other ranges.
  • the amount of the polytype 15R phase may be between 25% and 55%.
  • Example 14 For example, referring to Example 14, one will be able to predict that a cutting tool insert would exhibit good wear resistance, as it is fabricated by processing the ceramic material with high ratio of polytype 15R phase.
  • Cutting tools i.e., inserts were fabricated with the ceramic materials prepared according to Examples 10, 11 and 14 of [Table 1]. Each insert was subject to a test with Inconel 718 by a turning, at a speed of 740 m/min, moving speed of 0.1 mm/rev, and to a cutting depth of 1.5 mm and a cutting width of 20 mm. No cutting oil was used.
  • FIG. 8 shows a milling test result of a cutting tool according to an exemplary embodiment.
  • FIG. 8 is based on the life of a cutting tool of Example 10 which is used with ⁇ -sialon free of polytype 15R.
  • the life of a cutting tool fabricated with ⁇ -sialon without polytype 15R is 100
  • the life of a cutting tool fabricated with a ceramic material (Example 11) including 5.64% polytype 15R and ⁇ -sialon can be 104.
  • the life of the cutting tool fabricated with ⁇ -sialon without polytype 15R is 100
  • the life of a cutting tool fabricated with a ceramic material (Example 14) including 48.8% polytype 15R and ⁇ -sialon can be 266.
  • the cutting tool fabricated with a ceramic material of Example 14 with the higher ratio of polytype 15R exhibits longest life.
  • the cutting tool fabricated with the ceramic material of Example 14 of higher polytype 15R ratio exhibits higher wear resistance than the cutting tool fabricated with the ceramic material of Example 11 with lower polytype 15R ratio, and also exhibits better wear resistance than the cutting tool fabricated with the ceramic material of Example 10 which is free of polytype 15R.

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Abstract

A ceramic material according to an exemplary embodiment consists of β-sialon (Si(6-z)AlzOzN(8-z)) and polytype 15R and intergranular phase, and contains yittrium, in which the polytype 15R includes twin grains.

Description

CERAMIC MATERIAL AND CUTTING TOOLS MADE THEREOF
The present disclosure relates to a silicon nitride ceramic material having wear resistance and toughness suitable for machining heat resistant super alloy (HRSA), and a cutting tool made of the same.
The high hot hardness of a ceramic material allows the ceramic material for cutting tools to be an appropriate choice for machining a workpiece which has high hardness, high tensile strength and low thermal expansion at elevated temperature, and it is particularly suitable for a self-hardening material such as nickel- or cobalt-based material which is often used for the heat resistant super alloy (HRSA).
Many nitride silicon materials for cutting tools are fabricated using aluminum oxide Al2O3 as a sintering additive. Because aluminum and oxygen can replace the silicon and nitrogen in silicon nitride crystal structure respectively, these can form so-called "sialon" ceramic. The sialon ceramic consists of silicon, aluminum, oxygen and nitrogen (Si-Al-O-N) and can sometimes be additionally stabilized by cation (Me), in which Men+ may refer to a material having proper ion radius (r＜1.0Å) with a plurality of rare earth metals, and may be selected from lanthanide such as Y, Yb, Dy, Lu, Li, Ca, Mg, Sc, for example.
Referring to "Progress in SiAlON ceramics" by Izhevskyi V A, Genova L A, Bressiani J C, and Aldinger F (J. Eur. Ceram. Soc. 20, 2275 ~ 2295(2000)), among a large number of sialon phases detected and characterized, the main phase for use in cutting tools remains in α-sialon phase, i.e., in RxSi12 - (m＋n)Al(m＋n)OnN(16-n) (1.0 ＜m＜2.7; n＜1.2) state, in which R is one of the above-mentioned metals or the lantanoide having smaller ion radius than 1.0Å, and β-sialon is Si6 - zAlzOzN(8-z) (0 ＜z＜4.2).
During sintering, the materials such as silicon nitride, alumina, AlN or a number of materials such as 12H, 21R used as a sialon polyphase (or polytype) composition temporarily form a molten material with lanthanoid or metal, or with lantanoid oxide. From this molten material, α- and β-sialon phases (if Y is used as metal ion R described above), and possibly, different phases such as YAG, melilite, B-phase, 12H and so on are crystallized. After sintering, the intergranular phase among crystalline particles remains. The amount of the produced intergranular phase is influenced by the composition of the materials and sintering conditions used.
The metal ion can not only act to stabilize the α-sialon phase, but also act as a catalyst to form sialon crystals during sintering. It usually aids forming of elongated sialon particles in β-phase, but elongated α-sialon particles are also produced. (Refer to "Nucleation and Growth of the Elongated α-SiAlON" by Fang-Fang X, Shu-Lin W, Nordberg L O, Ekstrom T (J. Eur. Ceram. Soc. 17(13) 1631-1638 (1997)).
US 7,629,281 proposes a ceramic material comprising β-sialon, 12H, and intergranular amorphous or partly crystalline phase and yittrium.
[Prior Art Documents]
Korean Patent Publication No. 10-2008-0061314
An object of the present disclosure is to provide a silicon nitride ceramic material for a metal cutting tool, having wear resistance and toughness suitable for machining heat resistant super alloy (HRSA).
An object of the present disclosure is to provide a cutting tool made of a silicon nitrαide ceramic material for a metal cutting tool, which has wear resistance and toughness for machining heat resistant super alloy (HRSA).
The objectives that are intended to be addressed by the present disclosure are not limited to that mentioned above, and other objectives that are not mentioned above can be clearly understood to those skilled in the art based on the description provided below.
In order to achieve the objects mentioned above, a ceramic material according to an exemplary embodiment consists of β-sialon (Si(6-z)AlzOzN(8-z)) and polytype 15R and intergranular phase, and contains yittrium, in which the polytype 15R includes twin grains.
In the ceramic material according to an exemplary embodiment, the amount of the polytype 15R is between 25% and 55%, as measured as a ratio of the height in a Cu-Kα X-ray diffraction pattern of 15R peak at a 2θ value of 34° and the height in the same diffraction pattern of the β-sialon peak at a 2θ value of 33°.
Exemplary embodiments of the present disclosure will be described in detail below with reference to the description and the drawings.
According to exemplary embodiments of the present disclosure, a ceramic material is provided, which has wear resistance and toughness proper for use in a cutting tool to machine heat resistant super alloy (HRSA).
The above and other objects, features and advantages of the present disclosure will become more apparent to those of ordinary skill in the art by describing in detail exemplary embodiments thereof with reference to the accompanying drawings, in which:
FIG. 1 shows an X-ray diffraction pattern from a ceramic material according to an exemplary embodiment;
FIG. 2 is a Scanning Electron Microscope (SEM) micrograph of a ceramic material according to an exemplary embodiment;
FIG. 3 shows a variation of Vickers hardness (HV) according to ratio of polytype 15R;
FIG. 4 shows a variation of Rockwell hardness (HRa) according to ratio of polytype 15R;
FIG. 5 shows a variation of fracture toughness (KIC) according to ratio of polytype 15R;
FIG. 6 shows a variation of brittleness (BI) according to ratio of polytype 15R;
FIG. 7 shows a variation of wear resistance (RW) according to ratio of polytype 15R; and
FIG. 8 shows a milling test result of a cutting tool according to an exemplary embodiment.
The raw materials used for the preparation of a ceramic material according to an exemplary embodiment and ratios thereof are shown in [Table 1] below. Y2O3 content and MgO content, which include metal ions for use as a catalyst in the preparation of the ceramic material, are fixed at 4 wt%.
No Weight %　
Si3N4 MgO AlN Y2O3 Al2O3
1 69.99 　 7.46 4.000 18.55
2 69.99 0.500 7.46 3.500 18.55
3 66.73 　 10.3 4.000 18.97
4 63.47 　 13.14 4.000 19.39
5 60.2 　 15.99 4.000 19.81
6 56.94 　 18.83 4.000 20.23
7 53.67 　 21.68 4.000 20.65
8 50.41 　 24.52 4.000 21.07
9 63.54 　 9.31 4.000 23.15
10 63.54 0.500 9.31 3.500 23.15
11 60.62 　 12.05 4.000 23.33
12 57.69 　 14.8 4.000 23.51
13 54.76 　 17.55 4.000 23.69
14 48.9 　 23.05 4.000 24.05
15 45.97 　 25.8 4.000 24.23
Powder mixture mixed at wt% according to [Table 1] is added with methanol as a solvent, a dispersant and a binder, and milled with a ball mill for about 20 hr. The raw materials are milled as described above so that a slurry of the raw materials is prepared.
After milling to prepare slurry, the slurry is granulated through a spray dryer. Powder is obtained by passing the granulated raw materials through a sieve.
The obtained powder is compressed into a compact. The compact is subject to de-binding, and then sintered and densified during 2 hours of gas pressure sintering at 1680℃ ~ 1820℃.
[Table 2] below shows the ceramic material prepared from the Examples shown in [Table 1] by the procedures described above. Further, the prepared ceramic material was analyzed with the X-ray diffractography.
FIG. 1 shows an X-ray diffraction pattern from a ceramic material according to an exemplary embodiment. For reference, referring to FIG. 1, β represents β-sialon (Si6 - zAlzOzN(8-z)), and 15R represents polytype 15R phase. Further, FIG. 1 shows the X-ray diffraction pattern of Example 14 (No. 14) for an example.
No z value of β-SiAlON(substitution rate) ratio of 15R/beta(%)
Za Zc average
1 1.45 1.46 1.46 0
2 1.48 1.50 1.49 0
3 1.48 1.47 1.48 4.71
4 1.47 1.47 1.47 9.18
5 1.43 1.44 1.43 19.48
6 1.39 1.38 1.38 30.69
7 1.39 1.37 1.38 39.22
8 1.39 1.36 1.37 51.17
9 1.84 1.85 1.85 0
10 1.89 1.90 1.90 0
11 1.76 1.79 1.78 5.64
12 1.77 1.77 1.77 12.2
13 1.71 1.74 1.73 21.47
14 1.68 1.69 1.68 48.8
15 1.63 1.65 1.64 71.22
Referring to FIG. 1, it is noted that the ceramic material according to an exemplary embodiment includes β-sialon, but does not include α-sialon. Further, based on the peak around 34° and a plurality of satellite peaks shown in FIG. 1, it is understood that the ceramic material according to an exemplary embodiment includes the polytype 15R phase.
Further, based on the X-ray diffraction pattern as shown in FIG. 1, a z value of the β-sialon included in the ceramic material prepared according to Examples of the present disclosure can be determined.
Additionally, the amount of the polytype 15R phase can be determined based on the ratio of the height in a Cu-Kα X-ray diffraction pattern of 15R peak at a 2θ value (b) of 34°, and the ratio of the height in a Cu-Kα X-ray diffraction pattern of the β-sialon peak at a 2θ value (a) of 33°.
FIG. 2 is a Scanning Electron Microscope (SEM) micrograph of a ceramic material according to an exemplary embodiment. For reference, FIG. 2 is the SEM micrograph of a sample prepared from Example 14 (No. 14). As shown in FIG. 2, the ceramic material consists of β-sialon, polytype 15R phase, and intergranular phase between β-sialon and polytype 15R phase.
Additionally, referring to FIG. 2, it is noted that the polytype 15R phase includes crystal grains of bright bands and dark bands repeatedly stacked on one another. Such crystal grains may be the twin grains. Accordingly, it is understood that, in the ceramic material according to an exemplary embodiment, the polytype 15R phase may include twin grains.
Among the materials for a ceramic material, Example 2 and Example 10 that include MgO do not form polytype 15R phase. In other words, among Examples 1 to 15, the Examples that form the polytype 15R phase use Y2O3 as a catalyst.
Accordingly, the ceramic material according to an exemplary embodiment may consist of β-sialon, polytype 15R phase and intergranular phase between β-sialon and polytype 15R phase, and may contain yittrium (Y) which was included in the raw material. Further, in the ceramic material according to an exemplary embodiment, the polytype 15R phase may include twin grains.
<Evaluation 1>
Examples 1 to 16 were tested for Vickers hardness (HV), Rockwell hardness (HRa) and fracture toughness (KIC), as shown in [Table 3] below. Referring to [Table 3], the unit of the Vickers hardness (HV) is kgf/㎟, and the unit of fracture toughness (KIC) is Pa·m1/2.
No HV HRa KIC ratio of 15R/beta(%)
1 1535.4 93.8 3.5 0
2 1542.7 93.8 3.42 0
3 1536.8 93.8 3.53 4.71
4 1526.3 93.7 3.58 9.18
5 1515.6 93.7 3.54 19.48
6 1514.6 93.6 3.71 30.69
7 1514.1 93.5 3.69 39.22
8 1487.4 93.4 3.73 51.17
9 1489.5 93.8 3.2 0
10 1514.6 93.8 3.14 0
11 1502.1 93.6 3.29 5.64
12 1493.3 93.6 3.02 12.2
13 1494.6 93.6 3.24 21.47
14 1475.6 93.3 3.59 48.8
15 1469.1 93.2 3.39 71.22
Referring to [Table 3], the Vickers hardness (HV) was measured, by pressing with a square base diamond pyramid indenter consisting of a 136 degree included angle between opposite faces under 10kg load, and measuring a diagonal line of the concave portion. At this time, the descending speed of the indenter was 150㎛/s, and 15 seconds of indentation time was maintained.
For the Rockwell hardness (HRa) of [Table 3], a steel ball of a predetermined shape or a diamond cone-shaped indenter was used to exert an initial reference load, after which the load was increased to test load (60 kgf in the measuring of the present disclosure). The load was then returned to the initial reference load. The Rockwell hardness was then defined based on the difference of depths of the two indentations, i.e., the difference between the depth under reference loading and depth of the indentation.
The fracture toughness (KIC) in [Table 3] is measured using [Mathematical equation 1] suggested by Lawn B. R. and Fuller E. R. in "Equilibrium penny-like cracks in indentation fracture" (J. Mat. Sci. 12: 2016-2024(1975)).
[Mathematical equation 1]
Figure PCTKR2015012203-appb-I000001
where, P denotes indentation load (10 kg), and c is a length of crack.
FIG. 3 shows a variation of Vickers hardness (HV) according to ratio of polytype 15R. FIG. 4 shows a variation of Rockwell hardness (HRa) according to ratio of polytype 15R. FIG. 5 shows a variation of fracture toughness (KIC) according to ratio of polytype 15R.
Referring to FIGS. 3 and 4, the Vickers hardness (HV) or the Rockwell hardness (HRa) shows decreasing tendency as the ratio of polytype 15R increases.
However, referring to FIG. 5, except for Example 15, it is noted that the fracture toughness (KIC) exhibits an increasing tendency as the ratio of the polytype 15R increases.
Additionally, [Table 4] shows the brittleness index (BI) and wear resistance (RW) according to different ratios of polytype 15R.
No ratio of 15R/beta(%) BI(×103) Rw
1 0 4.30 0.66
2 0 4.42 0.65
3 4.71 4.27 0.66
4 9.18 4.18 0.67
5 19.48 4.20 0.67
6 30.69 4.00 0.69
7 39.22 4.02 0.69
8 51.17 3.91 0.70
9 0 4.56 0.63
10 0 4.73 0.61
11 5.64 4.47 0.64
12 12.2 4.85 0.60
13 21.47 4.52 0.63
14 48.8 4.03 0.69
15 71.22 4.25 0.66
Referring to [Table 4], the brittleness index (BI) is proportional to the Vickers hardness (HV), but is inversely proportional to the fracture toughness (KIC). [Mathematical equation 2] as below is used to obtain the brittleness index (BI) in [Table 4].
[Mathematical equation 2]
BI = HV/KIC
The wear resistance (RW) in [Table 4] is an index to the frictional wear excluding chemical wear, which is inversely proportional to the Vickers hardness (HV), but is proportional to the fracture toughness (KIC). Also notable is higher sensitivity to the variation of fracture toughness (KIC), than to the Vickers hardness (HV). [Mathematical equation 3] as below is used to obtain the wear resistance (RW) in [Table 4].
[Mathematical equation 3]
RW = KIC 3/4 / HV 0.5
FIG. 6 shows a variation of brittleness (BI) according to ratio of polytype 15R. FIG. 7 shows a variation of wear resistance (RW) according to ratio of polytype 15R.
Referring to [Table 4], and FIGS. 6 and 7, as the ratio of the polytype 15R phase increases, wear resistance shows increasing tendency, while brittleness index shows decreasing tendency. That is, as shown in FIG. 3, the Vickers hardness (HV) shows decreasing tendency as the ratio of the polytype 15R increases, and as shown in FIG. 5 (but excluding Example 15), the fracture toughness (KIC) shows increasing tendency as a ratio of the polytype 15R increases, which are similar to the tendencies shown in FIGS. 6 and 7.
More specifically, it is understood that a ceramic material having between 25% and 55% of a ratio of polytype 15R phase may have lower brittleness index, but have higher wear resistance than the ceramic materials including polytype 15R phase of other ranges.
In the ceramic material according to an exemplary embodiment, the amount of the polytype 15R phase may be between 25% and 55%.
For example, referring to Example 14, one will be able to predict that a cutting tool insert would exhibit good wear resistance, as it is fabricated by processing the ceramic material with high ratio of polytype 15R phase.
<Evaluation 2>
Cutting tools, i.e., inserts were fabricated with the ceramic materials prepared according to Examples 10, 11 and 14 of [Table 1]. Each insert was subject to a test with Inconel 718 by a turning, at a speed of 740 m/min, moving speed of 0.1 mm/rev, and to a cutting depth of 1.5 mm and a cutting width of 20 mm. No cutting oil was used.
The frequency of cycles of withstanding by each insert was recorded, until the flank wear depth (Vb) became 0.45 mm.
FIG. 8 shows a milling test result of a cutting tool according to an exemplary embodiment.
FIG. 8 is based on the life of a cutting tool of Example 10 which is used with β-sialon free of polytype 15R.
When the life of the cutting tool fabricated with β-sialon without polytype 15R is 100, the life of a cutting tool fabricated with a ceramic material (Example 11) including 5.64% polytype 15R and β-sialon can be 104.
Further, when the life of the cutting tool fabricated with β-sialon without polytype 15R is 100, the life of a cutting tool fabricated with a ceramic material (Example 14) including 48.8% polytype 15R and β-sialon can be 266.
As indicated by the milling test result of FIG. 8, it is notable that the cutting tool fabricated with a ceramic material of Example 14 with the higher ratio of polytype 15R exhibits longest life. In other words, it is understood that the cutting tool fabricated with the ceramic material of Example 14 of higher polytype 15R ratio exhibits higher wear resistance than the cutting tool fabricated with the ceramic material of Example 11 with lower polytype 15R ratio, and also exhibits better wear resistance than the cutting tool fabricated with the ceramic material of Example 10 which is free of polytype 15R.
The milling test result of FIG. 8 reveals that the tendency is in agreement with that exhibited by [Table 4] and FIG. 7.
Those with ordinary knowledge in the technical field of the present disclosure will be able to understand that the present disclosure can be embodied into different and more detailed modes, without departing from the technical concept or without modifying essential characteristics thereof. Accordingly, it will be understood that the exemplary embodiments described above are only illustrative, and should not be construed as limiting. While the scope of the present disclosure is represented by the claims accompanied below, the meaning and the scope of the claims, and all the modifications or modified forms that can be derived from the equivalent concepts will have to be interpreted as falling into the scope of the present disclosure.

Claims (3)

  1. A ceramic material consisting of β-sialon (Si(6-z)AlzOzN(8-z)), polytype 15R, and intergranular phase, and containing yittrium,
    wherein the polytype 15R comprises twin grains.
  2. The ceramic material according to claim 1, wherein an amount of the polytype 15R is between 25% and 55%, as measured as a ratio of a height in a Cu-Kα X-ray diffraction pattern of 15R peak at a 2θ value of 34° and a height in the same diffraction pattern of a β-sialon peak at a 2θ value of 33°.
  3. A cutting tool for machining a chip-forming metal, fabricated with a material according to claims 1 to 2.
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