Use of gradient layers and stress modifiers to fabricate composite constructs

• US 7,396,501 B2
• Filed: 08/27/2004
• Issued: 07/08/2008
• Est. Priority Date: 08/12/1994
• Status: Expired due to Fees

• Current Assignee: Diamicron, Inc.
• Original Assignee: Diamicron, Inc.
• Inventors: Gardinier, Clayton F., Pope, Louis M., Vail, Michael A., Pope, Bill J., Dixon, Richard H., Taylor, Jeffery K., Blackburn, Dean C., Medford, Troy, Carvajal, Victoriano
• Primary Examiner(s): LOPEZ, CARLOS N
• Application Number:
  US10/928,928
• Publication Number:
  US 20050146086A1
• Time in Patent Office: 1,411 Days
• Field of Search: 264/642, 264/643, 623/23.6, 623/23.53
• US Class Current: 264/642
• CPC Class Codes: A61F 2/30767 Special external or bone-contacting surface, e.g. coating for improving bone ingrowth
• CPC Class Codes: A61F 2/3094 Designing or manufacturing processes
• CPC Class Codes: A61F 2/32 for the hip
• CPC Class Codes: A61F 2/3662 Femoral shafts
• CPC Class Codes: A61F 2/3676 Distal or diaphyseal parts of shafts
• CPC Class Codes: A61F 2/442 Intervertebral or spinal discs, e.g. resilient non-disc-shaped intervertebral inflatable pockets A61F2/441; non-disc-shaped intervertebral fusion implants A61F2/4455
• CPC Class Codes: A61F 2/4425 made of articulated components
• CPC Class Codes: A61F 2002/30092 using shape memory or superelastic materials, e.g. nitinol
• CPC Class Codes: A61F 2002/30331 made by longitudinally pushing a protrusion into a complementarily-shaped recess, e.g. held by friction fit
• CPC Class Codes: A61F 2002/30392 Rotation
• CPC Class Codes: A61F 2002/30398 Sliding
• CPC Class Codes: A61F 2002/30433 using additional screws, bolts, dowels, rivets or washers e.g. connecting screws
• CPC Class Codes: A61F 2002/30451 soldered or brazed or welded
• CPC Class Codes: A61F 2002/30578 having apertures, e.g. for receiving fixation screws
• CPC Class Codes: A61F 2002/30649 Ball-and-socket joints
• CPC Class Codes: A61F 2002/30836 knurled
• CPC Class Codes: A61F 2002/30841 Sharp anchoring protrusions for impaction into the bone, e.g. sharp pins, spikes
• CPC Class Codes: A61F 2002/3085 with a threaded, e.g. self-tapping, bone-engaging surface, e.g. external surface
• CPC Class Codes: A61F 2002/30884 Fins or wings, e.g. longitudinal wings for preventing rotation within the bone cavity
• CPC Class Codes: A61F 2002/30904 serrated profile, i.e. saw-toothed
• CPC Class Codes: A61F 2002/30934 : Special articulating surfaces
• CPC Class Codes: A61F 2002/30968 : Sintering
• CPC Class Codes: A61F 2002/3097 : using laser
• CPC Class Codes: A61F 2002/30971 : Laminates, i.e. layered products
• CPC Class Codes: A61F 2002/3611 : Heads or epiphyseal parts of femur
• CPC Class Codes: A61F 2002/3631 : with an integral complete or partial peripheral collar or bearing shoulder at its base
• CPC Class Codes: A61F 2002/443 : having two transversal endplates and at least one intermediate component
• CPC Class Codes: A61F 2002/4631 : the prosthesis being specially adapted for being cemented
• CPC Class Codes: A61F 2210/0014 : using shape memory or superelastic materials, e.g. nitinol
• CPC Class Codes: A61F 2220/0025 : Connections or couplings between prosthetic parts, e.g. between modular parts; Connecting elements
• CPC Class Codes: A61F 2220/0033 : made by longitudinally pushing a protrusion into a complementary-shaped recess, e.g. held by friction fit
• CPC Class Codes: A61F 2220/0041 : using additional screws, bolts, dowels or rivets, e.g. connecting screws
• CPC Class Codes: A61F 2220/0058 : soldered or brazed or welded
• CPC Class Codes: A61F 2310/00017 : Iron- or Fe-based alloys, e.g. stainless steel
• CPC Class Codes: A61F 2310/00023 : Titanium or titanium-based alloys, e.g. Ti-Ni alloys
• CPC Class Codes: A61F 2310/00029 : Cobalt-based alloys, e.g. Co-Cr alloys or Vitallium
• CPC Class Codes: A61F 2310/00095 : Niobium or Nb-based alloys
• CPC Class Codes: A61F 2310/00131 : Tantalum or Ta-based alloys
• CPC Class Codes: A61F 2310/00149 : Platinum or Pt-based alloys
• CPC Class Codes: A61F 2310/00167 : Diamond or diamond-like carbon
• CPC Class Codes: A61F 2310/00269 : based on metal carbides
• CPC Class Codes: A61F 2310/00281 : containing silicon carbide
• CPC Class Codes: A61F 2310/00293 : containing a phosphorus-containing compound, e.g. apatite
• CPC Class Codes: A61F 2310/0058 : Coating made of diamond or of diamond-like carbon DLC
• CPC Class Codes: A61L 27/303 : Carbon
• CPC Class Codes: A61L 27/306 : Other specific inorganic materials not covered by A61L27/303 - A61L27/32
• CPC Class Codes: B22F 1/12 : Metallic powder containing non-metallic particles containing lubricating or binding agents or organic material B22F1/10
• CPC Class Codes: B22F 2207/01 : Composition gradients
• CPC Class Codes: B22F 2998/00 : Supplementary information concerning processes or compositions relating to powder metallurgy
• CPC Class Codes: B22F 2998/10 : Processes characterised by the sequence of their steps
• CPC Class Codes: B22F 3/12 : Both compacting and sintering by forging B22F3/17
• CPC Class Codes: B22F 7/02 : of composite layers B22F7/002 takes precedence
• CPC Class Codes: B29C 43/006 : Pressing and sintering powders, granules or fibres
• CPC Class Codes: B29L 2031/7532 : Artificial members, protheses
• CPC Class Codes: C04B 2235/3839 : Refractory metal carbides
• CPC Class Codes: C04B 2235/3856 : Carbonitrides, e.g. titanium carbonitride, zirconium carbonitride
• CPC Class Codes: C04B 2235/3886 : Refractory metal nitrides, e.g. vanadium nitride, tungsten nitride
• CPC Class Codes: C04B 2235/427 : Diamond
• CPC Class Codes: C04B 2235/5436 : micrometer sized, i.e. from 1 to 100 micron
• CPC Class Codes: C04B 2235/5445 : submicron sized, i.e. from 0,1 to 1 micron
• CPC Class Codes: C04B 2235/5472 : Bimodal, multi-modal or multi-fraction
• CPC Class Codes: C04B 35/52 : based on carbon, e.g. graphite
• CPC Class Codes: C22C 26/00 : Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes

Abstract

Use of gradient layers and stress modifiers in superhard constructs.

Claims

1. A method for making a sintered polycrystalline diamond compact comprising the steps of:

selecting a substrate containing a desired solvent metal,

placing a first gradient layer of diamond adjacent said substrate,

placing a second gradient layer of diamond adjacent said first gradient layer of diamond,

exposing the assembly of said substrate and said first and second gradient diamond layers to high pressure and temperature in a press,

sweeping said solvent metal from said substrate through said first and second gradient layers of diamond in order to solvate said diamond in said solvent metal and to then resolidify said gradient diamond layers and said substrate into a sintered polycrystalline diamond compact.

2. A method as recited in claim 1 further comprising the step of mixing solvent metal with a diamond feedstock and forming one of the gradient layers of diamond therefrom prior to sintering.

3. A method as recited in claim 1 wherein said solvent metal sweeps from said substrate through said diamond gradient layer as a wave front during sintering to quickly wet and dissolve said diamond.

4. A method as recited in claim 2 wherein the method comprises using only as much solvent metal is used as is necessary to precipitate diamond particle-to-particle bonding during sintering.

5. A method as recited in claim 1 wherein the method comprises using solvent metal sweeping from said substrate through said diamond to carry away impurities in said diamond.

6. A method as recited in claim 1 wherein the method comprises providing said diamond table with an optimized level of solvent metal in it due to improved sweep of solvent metal through the diamond during sintering, as compared to the sweep of solvent metal through the diamond when gradient layers of diamond are not use.

7. A method as recited in claim 1 wherein said solvent metal is cobalt.

8. A method as recited in claim 1 wherein said diamond gradient layers comprise diamond particles having a size primarily in the range of 1 to 40 microns.

9. A method as recited in claim 1 wherein said solvent metal is CoCrMo.

10. A method for making a sintered polycrystalline diamond compact comprising the steps of:

providing a first gradient layer of diamond,

placing a second gradient layer of diamond adjacent said first gradient layer of diamond,

providing a simulated substrate that provides a controlled release and limited supply of CoCrMo as a solvent metal,

exposing the assembly of said simulated substrate and first and second gradient diamond layers to high pressure and temperature in a press, and

sweeping said solvent metal from said simulated substrate through said second gradient layer of diamond in order to solvate said diamond in said solvent metal and then resolidify said first and second gradient diamond layers and said simulated substrate into a sintered polycrystalline diamond compact.

11. A method as recited in claim 10 wherein one of the first and second gradient layers of diamond comprises said limited supply of CoCrMo so as to form the simulated substrate and wherein said limited supply of CoCrMo solvent metal sweeps through the other gradient layer of diamond.

12. A method as recited in claim 10 wherein said step of providing a simulated substrate includes providing a mixture of Cr₃C₂, and CoCrMo in said first gradient layer of diamond.

13. A method as recited in claim 10 wherein said simulated substrate includes a mixture of diamond and CoCrMo.

14. A method as recited in claim 10 herein said simulated substrate includes a mixture of diamond and Cr₃C₂.

15. A method as recited in claim 10 further comprising the step of controlling the bulk modulus of gradient layers to control the overall dilatation of the construct during the sintering process.

16. A method as recited in claim 10 further comprising the step of adjusting the ratio of metal or carbides to diamond to reduce the CTE of an individual gradient layer.

17. A method as recited in claim 10 further comprising the step of creating residual stresses in the sintered polycrystalline diamond compact.

18. A method as recited in claim 10 further comprising the step of directing stress tensor vectors toward a desired direction in the sintered polycrystalline diamond compact.

19. A method as recited in claim 10 further comprising the step of reducing interface stresses between gradient layers of diamond.

20. A method as recited in claim 10 wherein each of said first and said second gradient layers of diamond include CoCrMo.

21. A method as recited in claim 10 where in one of said first and said second gradient layers of diamond includes Cr₃C₂ but the other does not.

22. A method as recited in claim 10 wherein said first gradient layer of diamond comprises at least 90% diamond by volume and wherein said second gradient layer of diamond comprises not more than 70% diamond by volume.

23. A method as recited in claim 10 further comprising the step of using gradient layers of diamond with solid layers of metal to match the bulk modulus to the CTE of various features of the construct to counteract dilatory forces encountered during the high temperature/high pressure phase of the sintering process.

24. A method as recited in claim 10 further comprising the step of balancing bulk modulus in the construct by selecting solvent metals with a compatible modulus of elasticity and balancing CTE by amount of diamond and carbides used in the gradient layers of diamond.

25. A method for making a sintered polycrystalline diamond compact comprising the steps of:

selecting a CoCr inner core,

placing a titanium layer around said inner core,

placing a first diamond outer layer against said titanium layer, the first diamond outer layer comprising CoCr as a sweep source of solvent metal,

placing a second diamond outer layer against said first diamond outer layer,

using said titanium layer as a diliatory source that offsets CTE from said solid CoCrMo inner layer and prevents it from pulling away from the titanium/CoCrMo interface as the sintering pressure and temperature goes from high pressure and high temperature to room temperature and ordinary barometric pressure,

exposing said inner core, said titanium layer, said first diamond outer layer, and said second diamond outer layer to high pressure and high temperature in order to sinter a polycrystalline diamond compact.

26. A method for making a sintered polycrystalline diamond compact comprising the steps of:

selecting a substrate containing a desired solvent metal,

said substrate having a CTE similar to that of diamond,

placing a first gradient layer of diamond adjacent said substrate,

placing a second gradient layer of diamond adjacent said first gradient layer of diamond,

exposing the assembly of said substrate and said first and second gradient layers of diamond to high pressure and temperature in a press, and

sweeping said solvent metal from said substrate through said first and second gradient layers of diamond in order to solvate said diamond in said solvent metal and then resolidify said gradient diamond layers and said substrate into a sintered polycrystalline diamond compact.

27. A method as recited in claim 26 further comprising the step of mixing a metal powder with at least one of said first and second gradient diamond layers to reduce stresses between diamond layers and thereby prevent their delamination from each other after sintering of the polycrystalline diamond compact.

28. A method as recited in claim 26 further comprising the steps of assembling a mold with said gradient diamond layers, and assembling a mold release between said diamond layers and said mold.

29. A method as recited in claim 26 further comprising the steps of placing a mold adjacent the second gradient layer of diamond and disposing an intermediate layer of material between the second gradient layer of diamond and the mold that prevents bonding of the polycrystalline diamond compact to the mold surface.

30. A method as recited in claim 26 further comprising the step of using a mold to form said sintered polycrystalline diamond compact that has a mold material that does not bond to the PDC under diamond sintering conditions.

31. A method as recited in claim 26 further comprising the step of using a mold to form the sintered polycrystalline diamond compact, the mold being made from a mold material that, when lowering the temperature and pressure following the sintering of the polycrystalline diamond compact the mold separates from the compact such that the mold either contracts away from the PDC where the PDC is generally concave, or expands away from the PDC wherein the PDC is generally convex.

32. A method as recited in claim 26 further comprising the step of using a mold that has a material that can also act as a source of solvent metal useful in the PDC synthesis process.

33. A method as recited in claim 26 further comprising the step of using a mold release system that has a negative shape of the desired geometry of the finished sintered polycrystalline diamond compact so that the mold surface contracts away from the final net concave geometry, and wherein the mold surface acts as a source of solvent-catalyst metal for the PDC synthesis process, and wherein the mold surface has poor bonding properties to PDCs and consequently creates conditions in which it is not difficult to remove the sintered polycrystalline diamond compact from the mold.

34. A method as recited in claim 26 further comprising the step of mixing low CTE material with a biocompatible metal substrate to reduce interfacial stresses between the diamond table and the substrate in a sintered polycrystalline diamond compact.

35. A method as recited in claim 34 wherein said low CTE material is diamond.

36. A method as recited in claim 34 wherein said low CTE material is selected from the group consiting of Carbides, Silicides, Oxynitrides, Nitrides, Oxides, Oxyborides, Borides, Oxycarbides, and Carbonitrides.

37. A method as recited in claim 26 further comprising creating creating residual stresses in the sintered polycrystalline diamond compact that cause the outer wear layer of diamond to be in compression to prevent delamination and crack propagation.

38. A method as recited in claim 37 wherein said residual stresses have stress tensors directed radially toward the center of the sintered polycrystalline diamond compact.

39. A method as recited in claim 26 further comprising the step of placing a third gradient layer of diamond adjacent said second gradient layer of diamond.

40. A method as recited in claim 39 further comprising the step of placing a fourth gradient layer of diamond adjacent said third gradient layer of diamond.

41. A method as recited in claim 26 further comprising the step of encapsulating said substrate with a refractory barrier prevent over saturation of the diamond during sintering.

42. A method as recited in claim 26 further comprising the step of using a substrate that includes a material selected from the group consisting of cemented tungsten carbide, niobium, nickel, stainless steel, steel, and ceramic.

43. A method as recited in claim 26 wherein said solvent metal includes TiCTiN.

44. A method as recited in claim 26 wherein said gradient layers are constructed to provide an interface gradient in the sintered polycrystalline diamond compact.

45. A method as recited in claim 26 wherein said gradient layers are constructed to provide an incremental gradient in the sintered polycrystalline diamond compact.

46. A method as recited in claim 26 wherein said gradient layers are constructed to provide a continuous gradient in the sintered polycrystalline diamond compact.