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Us 2011/0031034 A1 Illll Illlllll II Illlll Illll Illll IllllUS Illll20110031034A1 Illll Illll Illll Illll Illll Illll Illlll Illl Illl Illl (19) nited States (12) Patent Application Publication (10) Pub. No.: S 2011/0031034 A1 DiGiovanni et al. (43) Pub. Date: Feb. 10, 2011 (54) POLYCRYSTALLINE COMPACTS Publication Classification INCLUDING IN-SITU NUCLEATED GRAINS, (51) Int. (71. EARTH-BORING TOOLS INCLUDING SUCH E21B 10/46 (2006.01) COMPACTS, AND METHODS OF FORMING B32B 5/16 (2006.01) SUCH COMPACTS AND TOOLS B32B 3/26 (2006.01) BO1J 35/02 (2006.01) (75) Inventors: Anthony A. DiGiovanni, Houston, CO1B 31/06 (2006.01) TX (US); Danny E. Scott, B82 Y 40/O0 (2011.01) Montgomery, TX (US) (52) U.S. CI ....... 175/428; 428/221; 428/323; 428/312.2; 502/100; 423/446; 977/734 Correspondence Address: (57) ABSTRACT Traskbritt, P.C. / Baker Hughes, Inc. Baker Hughes, Inc. Polycrystalline compacts include hard polycrystalline mate- P.O. Box 2550 rials comprising in situ nucleated smaller grains of hard mate- Salt Lake City, UT 84110 (US) rial interspersed and inter-bonded with larger grains of hard material. The average size of the larger grains may be at least about 250 times greater than the average size of the in situ Assignee: BAKER HUGHES (73) nucleated smaller grains. Methods of forming polycrystalline INCORPORATED, Houston, TX compacts include nucleating and catalyzing the formation of (US) smaller grains of hard material in the presence of larger grains of hard material, and catalyzing the formation of inter-granu- (21) Appl. No.: 12/852,313 lar bonds between the grains of hard material. For example, nucleation particles may be mixed with larger diamond (22) Filed: Aug. 6, 2010 grains, a carbon source, and a catalyst. The mixture may be subjected to high temperature and high pressure to form in smaller diamond grains using the nucleation particles, the Related U.S. Application Data carbon source, and the catalyst, and to catalyze formation of (60) Provisional application No. 61/232,265, filed onAug. diamond-to-diamond bonds between the smaller and larger 7, 2009. diamond grains. 26 24 28 Patent Application Publication Feb. 10, 2011 Sheet 1 of 4 US 2011/0031034 A1 12 14 FIG. 1A i L-",. i r " FIG. 1B Patent Application Publication Feb. 10, 2011 Sheet 2 of 4 US 2011/0031034 A1 26 ? iiiiiiiiiiI iiiiiiiIII?/ FIG. 2 26 28 FIG. 3 Patent Application Publication Feb. 10, 2011 Sheet 3 of 4 US 2011/0031034 A1 46 24 Patent Application Publication Feb. 10, 2011 Sheet 4 of 4 US 2011/0031034 A1 I 10 FIG. 5 US 2011/0031034 A1 Feb. 10, 2011 POLYCRYSTALLINE COMPACTS diamond table may contribute to thermal damage in the dia- INCLUDING IN-SITU NUCLEATED GRAINS, mond table when the cutting element is heated during use, due EARTH-BORING TOOLS INCLUDING SUCH to friction at the contact point between the cutting element COMPACTS, AND METHODS OF FORMING and the formation. SUCH COMPACTS AND TOOLS [0007] Polycrystalline diamond compact cutting elements in which the catalyst material remains in the diamond table CROSS-REFERENCE TO RELATED are generally thermally stable up to a temperature of about APPLICATIONS seven hundred and fifty degrees Celsius (750° C.), although [0001] This application claims the benefit of U.S. Provi- internal stress within the cutting element may begin to sional Patent Application Ser. No. 61/232,265 filed Aug. 7, develop at temperatures exceeding about four hundred 2009, the disclosure of which is hereby incorporated herein degrees Celsius (400° C.) due to a phase change that occurs in by this reference in its entirety. cobalt at that temperature (a change from the "beta" phase to the "alpha" phase). Also beginning at about four hundred TECHNICAL FIELD degrees Celsius (400° C.), there is an internal stress compo- nent that arises due to differences in the thermal expansion of [0002] The present invention relates generally to polycrys- the diamond grains and the catalyst metal at the grain bound- talline compacts, to tools including such compacts, and to aries. This difference in thermal expansion may result in methods of forming such polycrystalline compacts and tools. relatively large tensile stresses at the interface between the diamond grains, and contributes to thermal degradation of the BACKGROUND microstructure when polycrystalline diamond compact cut- [0003] Earth-boring tools for forming wellbores in subter- ting elements are used in service. Differences in the thermal ranean earth formations generally include a plurality of cut- expansion between the diamond table and the cutting element ting elements secured to a body. For example, fixed-cutter substrate to which it is bonded further exacerbate the stresses earth-boring rotary drill bits (also referred to as "drag bits") in the polycrystalline diamond compact. This differential in include a plurality of cutting elements that are fixedly thermal expansion may result in relatively large compressive attached to a bit body of the drill bit. Similarly, roller cone and/or tensile stresses at the interface between the diamond earth-boring rotary drill bits may include cones that are table and the substrate that eventually lead to the deterioration mounted on bearing pins extending from legs of a bit body of the diamond table, cause the diamond table to delaminate such that each cone is capable of rotating about the bearing from the substrate, or result in the general ineffectiveness of pin on which it is mounted. A plurality of cutting elements the cutting element. may be mounted to each cone of the drill bit. [0008] Furthermore, at temperatures at or above about [0004] The cutting elements used in such earth-boring tools seven hundred and fifty degrees Celsius (750° C.), some of often include polycrystalline diamond compact (often the diamond crystals within the diamond table may react with referred to as "PDC") cutting elements, which are cutting the catalyst material causing the diamond crystals to undergo elements that include cutting faces of a polycrystalline dia- a chemical breakdown or conversion to another allotrope of mond material. Polycrystalline diamond material is material carbon. For example, the diamond crystals may graphitize at that includes inter-bonded grains or crystals of diamond the diamond crystal boundaries, which may substantially material. In other words, polycrystalline diamond material weaken the diamond table. Also, at extremely high tempera- includes direct, inter-granular bonds between the grains or tures, in addition to graphite, some of the diamond crystals crystals of diamond material. The terms "grain" and "crystal" may be converted to carbon monoxide and carbon dioxide. are used synonymously and interchangeably herein. [0009] In order to reduce the problems associated with [0005] Polycrystalline diamond compact cutting elements differences in thermal expansion and chemical breakdown of are formed by sintering and bonding together relatively small the diamond crystals in polycrystalline diamond cutting ele- diamond grains under conditions of high temperature and ments, so-called "thermally stable" polycrystalline diamond high pressure in the presence of a catalyst (such as, for compacts (which are also known as thermally stable products, example, cobalt, iron, nickel, or alloys and mixtures thereof) or "TSPs") have been developed. Such a thermally stable to form a layer or"table" ofpolycrystalline diamond material polycrystalline diamond compact may be formed by leaching on a cutting element substrate. These processes are often the catalyst material (e.g., cobalt) out from interstitial spaces referred to as high temperature/high pressure (or "HTHP") between the inter-bonded diamond crystals in the diamond processes. The cutting element substrate may comprise a table using, for example, an acid or combination of acids cermet material (i.e., a ceramic-metal composite material) (e.g., aqua regia). A substantial amount of the catalyst mate- such as, for example, cobalt-cemented tungsten carbide. In rial may be removed from the diamond table, or catalyst such instances, the cobalt (or other catalyst material) in the material may be removed from only a portion thereof. Ther- cutting element substrate may be swept into the diamond mally stable polycrystalline diamond compacts in which sub- grains during sintering and serve as the catalyst material for stantially all catalyst material has been leached out from the forming the inter-granular diamond-to-diamond bonds diamond table have been reported to be thermally stable up to between, and the resulting diamond table from, the diamond temperatures of about twelve hundred degrees Celsius grains. In other methods, powdered catalyst material may be (1,200° C.). It has also been reported, however, that such fully mixed with the diamond grains prior to sintering the grains leached diamond tables are relatively more brittle and vulner- together in a HTHP process. able to shear, compressive, and tensile stresses than are non- [0006] Upon formation of a diamond table using a HTHP leached diamond tables. In addition, it is difficult to secure a process, catalyst material may remain in interstitial spaces completely leached diamond table to a supporting substrate. between the grains of diamond in the resulting polycrystalline In an effort to provide cutting elements having diamond diamond table. The presence of the catalyst material in the tables that are more thermally stable relative to non-leached US 2011/0031034 A1 Feb. 10, 2011 2 diamond tables, but that are also relatively less brittle and of hard material in a hard polycrystalline material like that of vulnerable to shear, compressive, and tensile stresses relative FIGS. 1A and 1B in accordance with embodiments of meth- to fully leached diamond tables, cutting elements have been ods of the present invention; provided that include a diamond table in which the catalyst [0017] FIG. 3 is a simplified drawing of another composite material has been leached from a portion or portions of the nucleation particle that may be used to form in situ nucleated diamond table.
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