IP Library Granted Patent US 9,334,193
Granted Patent B2
US 9,334,193 · App. 13/579,472 · Granted May 10, 2016

Wear resistant member, and method for manufacturing the wear resistant member

Inventor: Minoru Takao (Yokohama, JP)
Assignees: KABUSHIKI KAISHA TOSHIBA; TOSHIBA MATERIALS CO., LTD.
C04B35/5935F16C33/043F16C33/12F16C33/32C04B2235/3206C04B2235/3208C04B2235/3217C04B2235/3225C04B2235/3232C04B2235/3241C04B2235/3244C04B2235/3251C04B2235/3256C04B2235/3258C04B2235/3272C04B2235/3865C04B2235/5409C04B2235/604C04B2235/656C04B2235/6562C04B2235/6567C04B2235/661C04B2235/72C04B2235/767C04B2235/77C04B2235/786C04B2235/788C04B2235/85C04B2235/96C04B2235/963F16C2206/60F16C2220/20Y10T428/24355
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Quick Facts
Patent No.
US 9,334,193
App. No.
13/579,472
Granted
May 10, 2016
Kind
B2
Abstract

A wear resistant member formed of ceramic sintered body mainly composed of silicon nitride, the ceramic sintered body containing 10 to 3500 ppm of an Fe component in terms of Fe element, more than 1000 ppm to 2000 ppm of a Ca component in terms of Ca element, and 1 to 2000 ppm of a Mg component in terms of Mg element, wherein a β-phase ratio of silicon nitride crystal grains is 95% or more, a maximum longer diameter of the silicon nitride crystal grains is 40 μm or less, Ca component existing in grain boundary phase is not detected by XRD (X-ray Diffraction method), and each of dispersions in Vickers hardness, fracture toughness and density of the wear resistant member is within a range of ±10%. According to this structure, there can be obtained a wear resistant member comprising a ceramic sintered body improved in grinding-work property in addition to an excellent wear resistant property.

Claims (49)

1. A wear resistant member comprising a ceramic sintered body, the ceramic sintered body comprising:

silicon nitride,

10 to 3,500 ppm by mass of a Fe component in terms of Fe element,

more than 1,000 ppm up to 2,000 ppm by mass of a Ca component in terms of Ca element,

1 to 2,000 ppm by mass of a Mg component in terms of Mg element,

1 to 5 mass % of a rare earth component in terms of a rare earth element, and

1 to 5 mass % of an Al component in terms of Al element;

wherein in the ceramic sintered body:

a β-phase ratio of silicon nitride crystal grains is 95% or more,

an average aspect ratio, which is defined as an average value of respective aspect ratios of silicon nitride crystal grains, is 2 or more,

a maximum longer diameter of the silicon nitride crystal grains in the ceramic sintered body is 40 μm or less, and

a grain boundary phase comprises amounts of the Ca component and Mg component that are below a detection limit of XRD (X-ray diffraction);

wherein the Ca component and the Mg component have been substantially changed into an amorphous form in the ceramic sintered body, and

wherein the ceramic sintered body comprises a ground surface having a surface roughness Ra of 1 μm or less; and

wherein the ceramic sintered body has a Vickers hardness of 1,430 or more, a fracture toughness of 6.0 MPa·m 1/2 or more and a density of 3.18 g/cm 3 or more; and

wherein the dispersion of the hardness, fracture toughness and density of the wear resistant member is within a range of ±10%.

2. The wear resistant member of claim 1 , wherein the ceramic sintered body further comprises 0.1 to 5 mass % of at least one element selected from the group consisting of Ti, Zr, Hf, W, Mo, Ta, Nb, and Cr.

3. The wear resistant member of claim 1 , wherein the ceramic sintered body further comprises 0.1 to 5 mass % of Hf.

4. The wear resistant member of claim 1 , wherein the ceramic sintered body has a density of 3.25 g/cm 3 or more.

5. The wear resistant member of claim 1 , wherein the material powder mixture comprises a silicon nitride material powder, a sintering agent powder, 100 to 2,000 ppm by mass of a Fe component in terms of Fe element, more than 1,100 ppm up to 1,600 ppm by mass of a Ca component in terms of Ca element, and 100 to 1,000 ppm by mass of an Mg component in terms of Mg element.

6. The wear resistant member of claim 1 , wherein the ceramic sintered body has a Vickers hardness of 1,430 or more, and a fracture toughness of 6.0 MPa·m 1/2 or more.

7. The wear resistant member of claim 1 that has a plate shape or a spherical shape.

8. A cutting tool, rolling jig, check ball of valve, engine, jig, tool rail, roller or other apparatus comprising the wear resistant member of claim 1 .

9. A wear resistant member produced by a method comprising:

preparing a material powder mixture comprising a silicon nitride material powder, a sintering agent powder, 10 to 3,500 ppm by mass of a Fe component in terms of elemental Fe, more than 1,000 ppm up to 2,000 ppm by mass of a Ca component in terms of elemental Ca, and 1 to 2,000 ppm by mass of a Mg component in terms of elemental Mg, 1 to 5 mass % of a rare earth component in terms of a rare earth element and 1 to 5 mass % of an Al component in terms of Al element;

molding the material powder mixture to form a molded body;

conducting a primary sintering operation on the molded body at a first sintering temperature of 1,600 to 1,950° C. to obtain a primary sintered body having a relative density of 80% or more and less than 98%;

cooling the primary sintered body wherein a cooling rate at a temperature range of the first sintering temperature to 1,400° C. is controlled to be greater than 100° C./hour;

conducting a secondary sintering operation on the primary sintered body at a second sintering temperature of 1,600 to 1,900° C. to obtain a secondary sintered body having a relative density of 98% or more;

cooling the secondary sintered body wherein a cooling rate at a temperature range of the second sintering temperature to 1,400° C. is controlled to be greater than 100° C./hour; and

grinding the ceramic sintered body so that a surface roughness Ra of the ceramic sintered body is 1 μm or less,

thereby forming a wear resistant member that comprises a ceramic sintered body comprising silicon nitride;

wherein in the ceramic sintered body:

a β-phase ratio of silicon nitride crystal grains is 95% or more,

an average aspect ratio, which is defined as an average value of respective aspect ratios of the silicon nitride crystal grains, that is 2 or more,

a maximum longer diameter of the silicon nitride crystal grains in the ceramic sintered body is 40 μm or less,

a grain boundary phase comprises amounts of the Ca component and Mg component that are below a detection limit of XRD;

wherein the ceramic sintered body has a \Tickers hardness of 1,430 or more, a fracture toughness of 6.0 MPa·m 1/2 or more and a density of 3.18 g/cm 3 or more;

wherein the dispersion of the hardness, fracture toughness and density of the wear resistant member is within a range of ±10%; and

wherein the Ca component and the Mg component have been substantially changed into an amorphous form in the ceramic sintered body.

10. The wear-resistant member of claim 9 , wherein said method further comprises adding Fe, Ca and/or Mg to the material powder mixture to bring levels of these components to 10 to 3,500 ppm by mass of an Fe component in terms of elemental Fe, more than 1,000 ppm up to 2,000 ppm by mass of a Ca component in terms of elemental Ca, and 1 to 2,000 ppm by mass of a Mg component in terms of elemental Mg.

11. The wear-resistant member of claim 9 , wherein said method further comprises selecting a material mixture that contains 10 to 3,500 ppm by mass of a Fe component in terms of elemental Fe, more than 1,000 ppm up to 2,000 ppm by mass of a Ca component in terms of elemental Ca, and 1 to 2,000 ppm by mass of a Mg component in terms of elemental Mg, without separately adding Fe, Ca or Mg to the silicon nitride material powder.

12. The wear-resistant member of claim 9 , wherein in said method the secondary sintering operation is performed by conducting a hot isostatic pressing (“HIP”) method on the primary sintered body.

13. The wear-resistant member of claim 1 that is produced by a primary sintering step that produces a sintered body having a relative density of 80 to less than 98% and a secondary sintering step that produces a sintered body that has a relative density of 98% or more.

14. The wear-resistant member of claim 1 that has an as-sintered surface that is easily ground compared to the surface of an otherwise identical wear-resistant member that has a grain boundary phase comprising amounts of the Ca component and Mg component that are above a detection limit of XRD (X-ray diffraction).

15. The wear-resistant member of claim 9 , wherein the rate of cooling the primary and/or secondary sintered body is controlled to be 120 to 500° C./hour.

16. The wear-resistant member of claim 9 , wherein the rate of cooling the primary and/or secondary sintered body is controlled to be 200 to 500° C./hour.

17. A set of wear-resistant members according to claim 1 , wherein the dispersion of the hardness, fracture toughness and density of the wear resistant members within the set is within a range of ±10%.

18. A set of wear-resistant members according to claim 9 , wherein the dispersion of the hardness, fracture toughness and density of the wear resistant members within the set is within a range of ±10%.

Assignments (4)
NUNC PRO TUNC ASSIGNMENT Recorded Feb 19, 2026
From: KABUSHIKI KAISHA TOSHIBA
To: TOSHIBA MATERIALS CO. LTD.
Reel/Frame 074940/0511 →
CHANGE OF NAME Recorded Feb 19, 2026
From: TOSHIBA MATERIALS CO. LTD.
To: NITERRA MATERIALS CO., LTD.
Reel/Frame 074941/0803 →
CHANGE OF ADDRESS Recorded Feb 19, 2026
From: KABUSHIKI KAISHA TOSHIBA
To: KABUSHIKI KAISHA TOSHIBA
Reel/Frame 074941/0846 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 16, 2012
From: TAKAO, MINORU
To: KABUSHIKI KAISHA TOSHIBA; TOSHIBA MATERIALS CO., LTD.
Reel/Frame 028799/0475 →
Priority Claims (1)
JP 2010-031455 · Feb 16, 2010 · national
Continuity (1)
Related Publication 20120321851A1 · Dec 20, 2012