Method for making fine diamond PDC

Information

  • Patent Grant
  • 8858665
  • Patent Number
    8,858,665
  • Date Filed
    Friday, September 23, 2011
    13 years ago
  • Date Issued
    Tuesday, October 14, 2014
    10 years ago
  • Inventors
  • Examiners
    • Parvini; Pegah
    Agents
    • Young Basile, P.C.
Abstract
A method for making a PDC cutting element for use in rock drilling containing sub-micron size diamond particles within the diamond body. Metals that do not readily dissolve carbon are employed to limit the dissolution and re-precipitation of fine diamond during the sintering of the diamond to the substrate.
Description
BACKGROUND

1. Field of the Invention


The present invention relates to a sintered polycrystalline diamond composite for use in rock drilling, machining of wear resistant materials, and other operations which require the high abrasion resistance or wear resistance of a diamond surface. Specifically, this invention relates to such bodies that include a polycrystalline diamond layer attached to a cemented carbide substrate via processing at ultrahigh pressures and temperatures.


2. Description of the Art


It is well known in the art to form a polycrystalline diamond cutting element by sintering diamond particles into a compact using a high pressure, high temperature (HPHT) press and a suitable catalyst sintering aid. Apparatus and techniques to accomplish the necessary sintering of the diamond particles are disclosed in U.S. Pat. No. 2,941,248 to Hall and U.S. Pat. No. 3,141,746 to DeLai.


U.S. Pat. No. 3,745,623 Wentorf et al. teaches sintering of the diamond mass in conjunction with tungsten carbide to produce a composite compact (PDC) in which the diamond particles are bonded directly to each other and to a cemented carbide substrate.


It has been proven challenging to produce a PDC with an average grain size of diamond less than about 1 micron. This sub-micron diamond powder is difficult to produce and handle during the processes involved in sintering a uniform diamond body and attaching it to a substrate. Additionally the property of this material to agglomerate and its low packing density produces a diamond compact containing re-precipitated diamond crystals that results in lowering the strength of the overall structure.


Attempts to overcome the difficulties in sintering sub-micron diamond have been proposed by Hara et al. in U.S. Pat. No. 4,303,442. These solutions, however, do not provide a PDC with enough uniformity in abrasion and impact resistance to be useful in drill bits for deep hole oil and gas drilling.


It is well known in the art to mix a catalyst with the diamond prior to HPHT sintering in order to provide a uniform mixture of these materials. This is especially helpful when working with very fine grain diamond that is difficult to penetrate with a catalyst when the fine grain diamond is densely compacted. A problem still exists after the catalyst melts since it dissolves the fine diamond grains which re-precipitate as larger diamond crystals in a non-uniform distribution throughout the sintered mass. U.S. Patent Application No. 20090178345 to Russell et al attempts to solve this problem by milling the diamond with a catalyst that itself has a very fine grain size. Unfortunately these finer size catalyst particles combine after melting and create the same problems of dissolving the very fine diamond crystals.


Thus, there remains a need to effectively control the grain size of very fine diamond used in the formation of polycrystalline diamond cutting tools.


SUMMARY

A method of making a PDC cutting element wherein a non-reactive material that exhibits low solubility for carbon is added to an unsintered mass of diamond crystals that fills an interconnected pore network during a high pressure, high temperature process to equalize the pressure between the pore network and the external mass of diamond crystals.


The diamond mass is a mixture of various size crystals in which some of the diamond crystals are smaller in size than the holes in the interconnected pore network.


The non-reactive material can be copper or an alloy of copper and a catalyst metal.


In another aspect, a method of making a PCD cutting element wherein a non-reactive material that exhibits low solubility for carbon is added to an unsintered mass of diamond crystal that fills an interconnected pore network during a high pressure, high temperature process to equalize the pressure between the pore network and the external mass of diamond crystals. The mixture is sintered to bond the mass to a substrate at high pressure and high temperature.


In another aspect, a method of making PCD cutting element includes the step of coating diamond crystals that are smaller in size than the pores of a interconnected pore network of a larger diamond mass with a non-reactive material that exhibit low solubility for carbon.





DETAILED DESCRIPTION OF THE DRAWING


FIG. 1 is an illustration of a compressed mass of diamond crystals showing the interconnected empty pore network.





DETAILED DESCRIPTION

The present method incorporates a metal, which is compatible with the catalyst or other sintering aid used to sinter a diamond mass, and does not dissolve carbon. The use of such material retards the dissolution of diamond crystals thereby eliminating recrystallization of very fine diamond into larger crystals that weaken the diamond body or alter its abrasion characteristics.


When loose diamond abrasive is compacted under high pressure there remains an empty or void pore network throughout the diamond mass. This is a result of the high compressive strength of diamond. Another characteristic of compressed diamond is its ability to form bridges within the compressed mass thereby creating areas of both low and high pressure within the mass.



FIG. 1 shows a small diamond crystal 1, which is contained in a large hole of a pore network 2, is not under pressure since the larger diamond crystals 3 do all of the work of supporting the structure under pressure. When the molten catalyst sweeps through the pore network it dissolves the small crystal and converts it to graphite. After the molten catalyst fills the pore network, the pressure is equalized so that dissolved carbon from the small crystal, which combines with carbon from other small crystals and from exposed faces of the larger diamond crystals, re-precipitates as a larger diamond crystal. If a metal or other material that doesn't react with diamond fills the empty pores, the pressure on the smaller crystals in the mass will increase to where diamond is the stable phase prior to catalyst sweep through. This retards the dissolution and re-precipitation of the smaller diamond crystals.


The metal can be added to the un-sintered mass of diamond as a powder by a milling or other procedure or it can be placed between the diamond mass and the substrate. The metal selected should have a melting point sufficiently below that of the catalyst so that it will fully penetrate the mass of diamond crystals prior to the sintering action that is to take place. As an example, copper that does not readily dissolve carbon can be used to infiltrate the diamond mass prior to the sweep through of a catalyst metal, such as cobalt, that has a higher melting point.


In an alternate method, the metal used to retard diamond dissolution is alloyed with a catalyst. For example, copper that does not readily dissolve carbon can be easily alloyed with catalytic metal, such as cobalt. Copper can be alloyed with many of the known catalyst metals and the percentage of each metal can be adjusted to control the reactivity with carbon in the diamond.


In another exemplary method, the fine diamond crystals may be coated with a non-reactive material that doesn't readily dissolve carbon. The coating may be thin enough so that it does not entirely fill the holes in the pore network of the larger mass. In this example, the coating serves to retard the dissolution of the fine diamond crystals into the catalyst used to sinter the diamond mass.

Claims
  • 1. A method of making a PDC cutting element comprising: adding a nonreactive material that exhibits low solubility for carbon to an unsintered mass of diamond crystals, the non-reactive material filling an interconnected pore network between the diamond crystals during a high-pressure high-temperature process to equalize the pressure between the pore network and an external mass, whereby the equalized pressure retards dissolution of the diamond crystals and reprecipitation of the diamond crystals into larger crystals during sintering.
  • 2. The method of claim 1 wherein the diamond mass is a mixture of various size diamond crystals wherein some of the diamond crystals are smaller than the holes in the interconnected pore network.
  • 3. The method of claim 1 wherein the nonreactive material is copper.
  • 4. The method of claim 1 wherein the nonreactive material is an alloy of copper and a catalyst metal.
  • 5. A method of making a PDC cutting element comprising: adding a nonreactive material exhibits low solubility for carbon to an unsintered mass of diamond crystals, to form a mixture, the non-reactive material filling an interconnected pore network between diamond crystals during a high-pressure high-temperature process to equalize the pressure between the pore network and an external mass, whereby the equalized pressure retards dissolution of the diamond crystals and reprecipitation of the diamond crystals into larger crystals during sintering; andsintering the mixture to bond the mass of diamond crystals to a substrate at high pressure and high temperature.
  • 6. The method of claim 5 wherein: the diamond crystal mass is a mixture of various size diamond crystals wherein some of the diamond crystals are smaller than the holes in the interconnected pore network.
  • 7. The method of claim 5 wherein the nonreactive material is copper.
  • 8. The method of claim 5 wherein the nonreactive material is an alloy of copper and a catalyst metal.
  • 9. A method of making a PDC cutting element comprising: coating diamond crystals that are smaller than pores of an interconnected pore network of a larger diamond crystal mass with a non-reactive material that exhibits low solubility for carbon, whereby the non-reactive material equalizes pressure between the pore network and the diamond crystals to retard dissolution of the diamond crystals and reprecipitation of the diamond crystals into larger crystals during sintering.
  • 10. The method of claim 9 wherein the diamond mass is a mixture of various size diamond crystals wherein some of the diamond crystals are smaller than the holes in the interconnected pore network.
  • 11. The method of claim 9 wherein the nonreactive material is copper.
  • 12. The method of claim 9 wherein the nonreactive material is an alloy of copper and a catalyst metal.
CROSS REFERENCE TO CO-PENDING APPLICATION

This application claims priority benefit of the U.S. Provisional Application Ser. Nos. 61/480,094 filed on Apr. 28, 2011 and 61/487,878 filed on May 19, 2011 in the name of R. Frushour, both of which are incorporated herein in their entirety.

US Referenced Citations (154)
Number Name Date Kind
2238351 Van Der Pyl Apr 1941 A
2941248 Hall Jun 1960 A
3083080 Bovenkerk Mar 1963 A
3134739 Cannon May 1964 A
3136615 Bovenkerk et al. Jun 1964 A
3141746 De Lai Jul 1964 A
3233988 Wentorf, Jr. et al. Feb 1966 A
3297407 Wentorf, Jr. Jan 1967 A
3423177 Bovenkerk Jan 1969 A
3574580 Stromberg et al. Apr 1971 A
3745623 Wentorf, Jr. et al. Jul 1973 A
4024675 Naidich et al. May 1977 A
4034066 Strong et al. Jul 1977 A
4042673 Strong Aug 1977 A
4063909 Mitchell Dec 1977 A
4073380 Strong et al. Feb 1978 A
4108614 Mitchell Aug 1978 A
4124690 Strong et al. Nov 1978 A
4151686 Lee et al. May 1979 A
4224380 Bovenkerk et al. Sep 1980 A
4247304 Morelock Jan 1981 A
4255165 Dennis et al. Mar 1981 A
4268276 Bovenkerk May 1981 A
4303442 Hara et al. Dec 1981 A
4311490 Bovenkerk et al. Jan 1982 A
4373593 Phaal et al. Feb 1983 A
4387287 Marazzi Jun 1983 A
4412980 Tsuji et al. Nov 1983 A
4481016 Campbell et al. Nov 1984 A
4486286 Lewin et al. Dec 1984 A
4504519 Zelez Mar 1985 A
4522633 Dyer Jun 1985 A
4525179 Gigl Jun 1985 A
4534773 Phaal et al. Aug 1985 A
4556407 Fecik et al. Dec 1985 A
4560014 Geczy Dec 1985 A
4570726 Hall Feb 1986 A
4572722 Dyer Feb 1986 A
4604106 Hall et al. Aug 1986 A
4605343 Hibbs, Jr. et al. Aug 1986 A
4606738 Hayden Aug 1986 A
4621031 Scruggs Nov 1986 A
4636253 Nakai et al. Jan 1987 A
4645977 Kurokawa et al. Feb 1987 A
4662348 Hall et al. May 1987 A
4664705 Horton et al. May 1987 A
4707384 Schachner et al. Nov 1987 A
4726718 Meskin et al. Feb 1988 A
4766040 Hillert et al. Aug 1988 A
4776861 Frushour Oct 1988 A
4792001 Zijsling Dec 1988 A
4793828 Burnand Dec 1988 A
4797241 Peterson et al. Jan 1989 A
4802539 Hall et al. Feb 1989 A
4807402 Rai Feb 1989 A
4828582 Frushour May 1989 A
4844185 Newton, Jr. et al. Jul 1989 A
4861350 Phaal et al. Aug 1989 A
4871377 Frushour Oct 1989 A
4899922 Slutz et al. Feb 1990 A
4919220 Fuller et al. Apr 1990 A
4940180 Martell Jul 1990 A
4943488 Sung et al. Jul 1990 A
4944772 Cho Jul 1990 A
4976324 Tibbitts Dec 1990 A
5011514 Cho et al. Apr 1991 A
5027912 Juergens Jul 1991 A
5030276 Sung et al. Jul 1991 A
5092687 Hall Mar 1992 A
5116568 Sung et al. May 1992 A
5127923 Bunting et al. Jul 1992 A
5133332 Tanaka et al. Jul 1992 A
5135061 Newton, Jr. Aug 1992 A
5176720 Martell et al. Jan 1993 A
5186725 Martell et al. Feb 1993 A
5199832 Meskin et al. Apr 1993 A
5205684 Meskin et al. Apr 1993 A
5213248 Horton et al. May 1993 A
5236674 Frushour Aug 1993 A
5238074 Tibbitts et al. Aug 1993 A
5244368 Frushour Sep 1993 A
5264283 Waldenstrom et al. Nov 1993 A
5337844 Tibbitts Aug 1994 A
5370195 Keshavan et al. Dec 1994 A
5379853 Lockwood et al. Jan 1995 A
5439492 Anthony et al. Aug 1995 A
5451430 Anthony et al. Sep 1995 A
5464068 Najafi-Sani Nov 1995 A
5468268 Tank et al. Nov 1995 A
5496638 Waldenstrom et al. Mar 1996 A
5505748 Tank et al. Apr 1996 A
5510193 Cerutti et al. Apr 1996 A
5523121 Anthony et al. Jun 1996 A
5524719 Dennis Jun 1996 A
5560716 Tank et al. Oct 1996 A
5607024 Keith et al. Mar 1997 A
5620382 Cho et al. Apr 1997 A
5624068 Waldenstrom et al. Apr 1997 A
5667028 Truax et al. Sep 1997 A
5672395 Anthony et al. Sep 1997 A
5718948 Ederyd et al. Feb 1998 A
5722499 Nguyen et al. Mar 1998 A
5776615 Wong et al. Jul 1998 A
5833021 Mensa-Wilmot et al. Nov 1998 A
5855996 Corrigan et al. Jan 1999 A
5897942 Karner et al. Apr 1999 A
5921500 Ellis et al. Jul 1999 A
5954147 Overstreet et al. Sep 1999 A
5981057 Collins Nov 1999 A
6009963 Chaves et al. Jan 2000 A
6030595 Sumiya et al. Feb 2000 A
6050354 Pessier et al. Apr 2000 A
6063333 Dennis May 2000 A
6123612 Goers Sep 2000 A
6126741 Jones et al. Oct 2000 A
6202770 Jurewicz et al. Mar 2001 B1
6248447 Griffin et al. Jun 2001 B1
6269894 Griffin Aug 2001 B1
6298930 Sinor et al. Oct 2001 B1
6344149 Oles Feb 2002 B1
6401845 Fielder Jun 2002 B1
6443248 Yong et al. Sep 2002 B2
6443249 Beuershausen et al. Sep 2002 B2
6460631 Dykstra et al. Oct 2002 B2
6544308 Griffin et al. Apr 2003 B2
6562462 Griffin et al. May 2003 B2
6582513 Linares et al. Jun 2003 B1
6585064 Griffin et al. Jul 2003 B2
6589640 Griffin et al. Jul 2003 B2
6592985 Griffin et al. Jul 2003 B2
6601662 Matthias et al. Aug 2003 B2
6681098 Pfenninger et al. Jan 2004 B2
6739214 Griffin et al. May 2004 B2
6749033 Griffin et al. Jun 2004 B2
6797326 Griffin et al. Sep 2004 B2
6811610 Frushour et al. Nov 2004 B2
6846341 Middlemiss Jan 2005 B2
6852414 Frushour Feb 2005 B1
6861137 Hughes et al. Mar 2005 B2
6878447 Griffin et al. Apr 2005 B2
7000715 Sinor et al. Feb 2006 B2
7070635 Frushour Jul 2006 B2
7316279 Wiseman et al. Jan 2008 B2
7517588 Frushour Apr 2009 B2
7595110 Frushour Sep 2009 B2
7757791 Belnap et al. Jul 2010 B2
20040062928 Raghavan et al. Apr 2004 A1
20050115744 Griffin et al. Jun 2005 A1
20080115421 Sani May 2008 A1
20080223623 Keshavan et al. Sep 2008 A1
20090152018 Sani Jun 2009 A1
20100032006 Basol Feb 2010 A1
20110083908 Shen et al. Apr 2011 A1
20110088954 Digiovanni et al. Apr 2011 A1
Foreign Referenced Citations (26)
Number Date Country
061954 Dec 1980 EP
0300699 Jan 1989 EP
0329954 Aug 1989 EP
0462091 Dec 1991 EP
0462955 Dec 1991 EP
0480895 Apr 1992 EP
0500253 Aug 1992 EP
0595630 May 1994 EP
0595631 May 1994 EP
0612868 Aug 1994 EP
0617207 Sep 1994 EP
0671482 Sep 1995 EP
0787820 Aug 1997 EP
0860515 Aug 1998 EP
1190791 Mar 2002 EP
2048927 Apr 2009 EP
2048927 Dec 1980 GB
2261894 Jun 1993 GB
2268768 Jan 1994 GB
2323110 Sep 1998 GB
2323398 Sep 1998 GB
59219500 Dec 1984 JP
9323204 Nov 1993 WO
9634131 Oct 1996 WO
0028106 May 2000 WO
2004022821 Mar 2004 WO
Related Publications (1)
Number Date Country
20120272583 A1 Nov 2012 US
Provisional Applications (2)
Number Date Country
61480094 Apr 2011 US
61487878 May 2011 US