Ceramic and process for the continuous sintering thereof

• US 6,471,734 B1
• Filed: 07/09/1998
• Issued: 10/29/2002
• Est. Priority Date: 07/09/1998
• Status: Expired due to Term

• Current Assignee: Kennametal Incorporated
• Original Assignee: Kennametal Incorporated
• Inventors: Yeckley, Russell L.
• Primary Examiner(s): DERRINGTON, JAMES H
• Application Number:
  US09/112,639
• Time in Patent Office: 1,573 Days
• Field of Search: 264/643, 264/652, 264/669, 264/670, 264/674, 264/683, 513/07, 513/09
• US Class Current: 51/307
• CPC Class Codes: C04B 2235/3206 Magnesium oxides or oxide-forming salts thereof
• CPC Class Codes: C04B 2235/3217 Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
• CPC Class Codes: C04B 2235/3225 Yttrium oxide or oxide-forming salts thereof
• CPC Class Codes: C04B 2235/36 Glass starting materials for making ceramics, e.g. silica glass
• CPC Class Codes: C04B 2235/3839 Refractory metal carbides
• CPC Class Codes: C04B 2235/3843 Titanium carbides
• CPC Class Codes: C04B 2235/3847 Tungsten carbides
• CPC Class Codes: C04B 2235/3856 Carbonitrides, e.g. titanium carbonitride, zirconium carbonitride
• CPC Class Codes: C04B 2235/3865 Aluminium nitrides
• CPC Class Codes: C04B 2235/3869 Aluminium oxynitrides, e.g. AlON, sialon
• CPC Class Codes: C04B 2235/3873 Silicon nitrides, e.g. silicon carbonitride, silicon oxynitride
• CPC Class Codes: C04B 2235/3878 Alpha silicon nitrides
• CPC Class Codes: C04B 2235/3886 Refractory metal nitrides, e.g. vanadium nitride, tungsten nitride
• CPC Class Codes: C04B 2235/3895 Non-oxides with a defined oxygen content, e.g. SiOC, TiON
• CPC Class Codes: C04B 2235/5244 Silicon carbide
• CPC Class Codes: C04B 2235/661 Multi-step sintering
• CPC Class Codes: C04B 2235/766 Trigonal symmetry, e.g. alpha-Si3N4 or alpha-Sialon
• CPC Class Codes: C04B 2235/767 Hexagonal symmetry, e.g. beta-Si3N4, beta-Sialon, alpha-SiC or hexa-ferrites
• CPC Class Codes: C04B 2235/77 Density
• CPC Class Codes: C04B 2235/80 Phases present in the sintered or melt-cast ceramic products other than the main phase
• CPC Class Codes: C04B 2235/85 : Intergranular or grain boundary phases
• CPC Class Codes: C04B 2235/96 : Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
• CPC Class Codes: C04B 35/10 : based on aluminium oxide
• CPC Class Codes: C04B 35/117 : Composites
• CPC Class Codes: C04B 35/119 : with zirconium oxide
• CPC Class Codes: C04B 35/48 : based on zirconium or hafnium oxides, zirconates, zircon or hafnates
• CPC Class Codes: C04B 35/56 : based on carbides or oxycarbides containing free metal binder C22C29/00
• CPC Class Codes: C04B 35/58 : based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides containing free binder metal C22C29/00
• CPC Class Codes: C04B 35/58021 : based on titanium carbonitrides
• CPC Class Codes: C04B 35/584 : based on silicon nitride
• CPC Class Codes: C04B 35/597 : based on silicon oxynitride, e.g. SIALONS
• CPC Class Codes: C04B 35/64 : Burning or sintering processes C04B33/32 takes precedence ; powder metallurgy B22F
• CPC Class Codes: C04B 41/009 : characterised by the material treated
• CPC Class Codes: C04B 41/4529 : applied from the gas phase
• CPC Class Codes: C04B 41/5025 : with ceramic materials copper oxide or solid solutions thereof C04B41/5074
• CPC Class Codes: C04B 41/5031 : Alumina
• CPC Class Codes: C04B 41/5061 : Titanium carbide
• CPC Class Codes: C04B 41/5068 : Titanium nitride
• CPC Class Codes: C04B 41/81 : Coating or impregnation
• CPC Class Codes: C04B 41/87 : Ceramics
• CPC Class Codes: F27B 9/243 : Endless-strand conveyor

Abstract

A continuous process for the manufacture of a ceramic sintered compact wherein the process comprises the steps of: forming a green compact from a powder mixture comprising a first component comprising compounds which contain elements of silicon, aluminum, oxygen and nitrogen; and the powder mixture further comprising a second component comprising a compound of at least one element selected from the group consisting of yttrium, scandium, cerium, lanthanum and the metals of the lanthanide series, and the second component comprising between 0.1 and 10 weight percent of the powder mixture; heat treating the green compact wherein the heat treatment comprises continuously passing the green compact through at least one heating zone so as to produce a sintered compact.

Claims

1. A continuous process for the manufacture of a ceramic sintered cutting insert body wherein the process comprises the steps of:

forming a green compact from a powder mixture comprising a first component comprising compounds which contain elements of silicon, aluminum, oxygen and nitrogen; and

the powder mixture further comprising a second component comprising a compound of at least one element selected from the group consisting of yttrium, scandium, cerium, lanthanum and the metals of the lanthanide series, and the second component comprising between 0.1 and 10 weight percent of the powder mixture;

heat treating the green compact wherein the heat treatment comprises continuously passing the green compact through at least one heating zone so as to produce the sintered cutting insert body, and wherein the one heating zone is at a temperature of greater than or equal to 1760 degrees Centigrade; and

wherein the sintered cutting insert body comprising SiAlON grains and an intergranular phase disposed between the SiAlON grains wherein the intergranular phase comprising glass pockets having a uniform distribution.

2. The process according to claim 1 wherein the ceramic material comprising a two-phase composite of alpha′

-SiAlON phase and beta′

-SiAlON phase, and a glassy phase; and

wherein the alpha′

-SiAlON phase ranges from 10 to 70 weight percent of the ceramic material, the beta′

-SiAlON phase ranges from 20 to 90 weight percent of the ceramic material, and the glassy phase ranges from 0.1 to 10 weight percent of the ceramic material.

3. The process according to claim 2 wherein the glassy phase may also contain a crystalline phase from the group consisting of YAG, YAM, N-YAM, and Y-N-α

-Wollastonite.

4. The process according to claim 2 wherein the ceramic material has the following physical properties:

a fracture toughness K_IC between about 5.93 and about 6.69 MPa m^½

, a hardness of between about 15.68 and about 16.30 GPa, and a density of between about 3.24 and about 3.26 grams per cubic centimeter.

5. The process according to claim 2 wherein the beta′

-SiAlON phase has the formula Si_6-zAl_zO_zN_8-z wherein z ranges between 0.38 and 1.5.

6. The process according to claim 5 wherein z is equal to about 0.8.

7. The process according to claim 1 wherein the heating zone is at a temperature between 1760°

C. and about 1800°

C. and the green compact is in the heating zone for a time between about sixty minutes and one hundred twenty minutes.

8. The process according to claim 1 wherein the forming step comprises:

milling the powder components;

agglomerating the powder components with lubricant; and

compacting the luburicant-agglomerated powder mixture into the green compact.

9. The process according to claim 8 wherein prior to the heat treating step, there is the step of delubing the green compact.

10. The process according to claim 9 wherein the green compact moves continuously from the delubing step to the heat treating step.

11. The process according to claim 1 wherein prior to the heat treating step, the green compact is placed in a container without any setting powder;

and the container carrying the green compact is placed on a belt which passes the container and green compact through the one heating zone.

12. The process according to claim 11 wherein the belt moves at a linear speed so as to control the duration of the green compact in the one heating zone.

13. The process according to claim 1 wherein the heat treatment further comprises subjecting the green compact to one atmosphere of flowing nitrogen.

14. The process according to claim 2 wherein the SiAlON grains comprises at least 50 volume percent of the ceramic;

wherein the ceramic has lass than 1 volume percent porosity;

wherein at least 70 volume percent of the SiAlON is beta′

-SiAlON phase and the intergranular phase forms 5 to 15 volume percent of the ceramic; and

wherein the beta-SiAlON phase has a Z value of greater than 0.4 but less than 4.

15. The process according to claim 14 wherein the Z value of the beta′

-SiAlON phase is about 3.

16. The process according to claim 14 wherein the ceramic material has the following physical properties:

a fracture toughness K_IC between about 5.70 and about 6.01 MPa m^½

, a hardness of between about 14.66 and about 15.10 GPa, and a density of between about 3.18 and about 3.19 grams per cubic centimeter.

17. The process according to claim 14 wherein at least ninety percent of the glass pockets have a major dimension being less than or equal to one micron.

18. The process according to claim 14 wherein the beta′

-SiAlON phase comprises at least about 85 volume percent of the SiAlON.

19. The process according to claim 14 wherein the beta′

-SiAlON phase comprises about 100 volume percent of the SiAlON.

20. The process according to claim 14 wherein the ceramic material includes one or refractory materials selected from the group consisting of titanium nitride, titanium carbonitride, titanium carbide, hafnium nitride, hafnium carbonitride, hafnium carbide, zirconium nitride, zirconium carbonitride, and zirconium carbide.

21. The process according to claim 1 wherein the sintered compact does not have a surface reaction layer.

22. The process according to claim 1 wherein the sintered compact has a surface reaction layer with a depth of no greater than 0.005 inches.

23. The process according to claim 1 further including the step of treating the sintered cutting insert body to form a cutting insert.

24. The process according to claim 23 further including the step of coating at least a portion of the cutting insert with a refractory coating.

25. The process according to claim 24 wherein the refractory coating is selected from the group consisting of alumina, titanium nitride and titanium carbonitride.

26. The process according to claim 14 wherein z is equal to about 0.4.

27. The process according to claim 1 wherein the heat treating step includes continuously passing the green compact through at least two heating zones so as to form the sintered compact, and wherein each one of the heating zones is at a temperature greater than 1760 degrees Centigrade.

28. The process according to claim 27 wherein one of the heating zones is at a temperature of about 1800 degrees Centigrade.

29. The process according to claim 1 wherein the compounds that comprise the first component include silicon nitride aluminum nitride and alumina.

30. The process according to claim 1 wherein the sintered cutting insert body having an as-molded rake face and an as-molded flank face, and the rake face intersecting with the flank face to form a cutting edge at the intersection, and the cutting insert body having at least one of the as-molded rake face and the as-molded flank face does not have a surface reaction layer.

31. The process according to claim 30 wherein at least one of the as-molded rake face and as-molded flank face has a surface reaction layer to a depth of no greater than 0.005 inches.

32. The process according to claim 2 further including the step of coating the sintered cutting insert body.

33. The process according to claim 2 wherein the sintered cutting insert body comprises:

a substrate comprising a two-phase composite of alpha′

-SiAlON and beta′

SiAlON, and a glassy phase;

the substrate presenting a surface, the substrate having a surface region extending inwardly from the surface, and the substrate having a bulk region beneath the surface region; and

the surface region having a higher alpha′

-SiAlON content than the bulk region.

34. The process according to claim 33 wherein the content of alpha′

-SiAlON in the surface region is between about two hundred percent to about five hundred percent greater than the alpha′

-SiAlON content in the bulk region.

35. The process according to claim 33 wherein the alpha′

-SiAlON content in the surface region ranges between about 57 weight percent and about 92 weight percent, and the alpha′

-SiAlON content in the bulk region comprises about 20 weight percent.

36. The process according to claim 33 wherein the surface region includes beta′

-SiAlON, and the beta′

-SiAlON content in the surface region being less than the beta′

-SiAlON content in the bulk region.