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‘US 2008) 1 48653. cu») United States cz) Patent Application Publication — co) Pub. No.: US 2008/0148653 Al Bauer et al. (43) Pub. Date Jun, 26, 2008 (54) SUBMICRON ALPHLA ALUMINA 1 Related TEMPERATURE BONDED ABRASIVES Application Data (60) Provisional application No, 60(870,740, ile on Dee. (75) Inventors: Ralph Bauer, Niagara alls (CA): eae Margaret L. Skowron, Nisgara Publication Classification Falls, NY ( 5 G1) Inve, Comespondence Address BUD 300 (2006.01) LARSON NEWMAN ABEL POLANSKY & — (52) US.Cl 51309 LP. : TCOURTYARD DRIVE, SUITE 200") ABSTRACT AUSTIN, TX 78730 A high temperature bonded abrasive inchades alumina aba sve grits, and a vitreous bond matrix in which the alumina (73) Assignce: SAINEGOBAIN CERAMICS & —_abrasivegrts are distribted, the vtreousbond matrix having PLASTICS, INC, Woreest ‘cue temperature not less than 1000” C, The alumina ab (ws) ive grits include polycrystalline alpha alumina having a fine erystalline mirosteuctre characterized by an alpha alumina Appl.No: 11984,735 average domain size not greater than SO0 am, and the alumina abrasive grits futher include a pinning agent tat is a dis File Dee. 12,2007 persed phase in the polyerystlline alphs alumina US 2008/0148653 Al SUBMICRON ALPHA ALUMINA HIGH. ‘TEMPERATURE BONDED ABRASIVES ‘CROSS REFERENCE TO RELATED "APPLICATIONS, {0001} The present application elsims priority from US. Provisional Patent Application No. 60/870, 740, fled Dec. 19 2006, entitled "SUBMICRON ALPHA ALUMINA HIGH TEMPERATURE BONDED ABRASIVES®, naming inven ‘ors Ralph Bauer and Margaret L, Skovsron, which appli tion is incorporated by reference herein i its entirety. BACKGROUND [0002] 1. Field ofthe Disclosure [0003] Aspects of the present invention are generally slirected to high temperature bonded abrasive tools and come ponents, particularly, high temperature Bonded abrasives that Incomporate fine microstructure alumina abrasive gris. [0004] 2. Description of the Related Ar 0005) High perfomance abrasive materials and compo- rents have Tong bees used in various indistal-machining applications, inctuding lapping/grindng, in which bulk mate- ial removal is executed, to fe polishing, in which fine ‘micron and submicron surface integularties are addressed. Typical materials that undergo such machining operations include various ceramics, lasses, glass-ceramics, metals and imetalalloys. Abrasives may tke on any one of various fons, such as fse abrasives as in an abrasive shury in which loose abrasive particles in suspension are used! for machining. Altematively abrasives may take the form of fixed abrasive, such asa coated abrasive or a bonds! abrasive, Coated abe fives are generally categorized as abrasive components fa jing an underlying substrate o Which abrasive grits or grains are adhered therto through a series of make coats and size ‘oats. Bonded abrasives typivally donot have an underlying Substrate and are formed of integral siniture of abrasive tits that are bonded together via a matrix bonding materi 10006] Sta of dae ar bonded abrasives ake advantage of vitreous bonding material, such as siliea-baed glass bond: ing matrices, Altemativey, specialized honded abrasives for ‘certain applications incorporate superabrasive ais, such as ‘cubic boron carbide and diamond, and may be integrally bonded through the use of a metal alloy bond max. 10007] While bonded abrasives have continued to undergo ‘development in recent years, particular attention hiss been pid high temperature bonded abresives that uilize a bond- {ng matex formed of a vitreous material. An example of & high temperature honded abrasive component is described ia US. Pat. No. $282,875. While state of the art high temipera- ture bonded abrasive components have improved perfor- mance and durability, a need continues to exist in the at for Jurther improved components, SUMMARY, 10008] According to one aspect, high temperature bonded abrasive is provided that includes alumina abrasive grits and ‘a vitveous Bond matrix in which the abrasive pits are distrib ted, The vitreous bond matrix has high temperature proper tis, inclutinga.cure temperature no Tess than about 1000°C. ‘The alumina abrasive grits comprise polycrystalline c-ali- ‘ming having a fine crystalline microstructure characterized by an ccalumina average domain size not greater than S00 1am. The alumina abrasive prits futher comprise a pinning Jun. 26, 2008 ‘agent, the pinning agent comprising a dispersed phase i polyerystalline -lumina phise [0009] According to another aspect, » high temperature ‘bonded abrasive is provided that includes alumina abrasive arts and vitreous bond matix in which the gris are distib- ‘uted. The vteeous bond maitx has cute temperatre not less than 1000" C. The alumina abrasive grits comprise polyerys- ‘alline c-alumina having a fine crystalline microstructure characterized by an average domain size of not greater than 300 nm, Further, the aluaiina abrasive gris eonipise a pin- fing dgent including at least a zirconium oxide phase di persed inthe polyerystalline a-alumina phase. [0010] In addition, a method for forming a high tempera ture bonded abrasive is provided, The method cals for form- ‘ng fine crystalline microstructure c-aumina abrasive grits by heat-treating c-alumina precursor containing a pinning ‘agent ata temperature not less than 1350° C. A shaped body is then formed containing the c-alumina grits and a vitreous ‘bond matrix material. Further, heat treatment of the sbapod body is earried out ata eure temperature not less than 1000° Coad above the melting point of the vitreous bond matrix ‘material. The alumina abrasive prits have an average erystal- line domsin size not greater than about 300 nm after be tecating, DESCRIPTION OF THE EMBODIMENTS [011] According to an embodiment, high-temperature bonded abrasive inchudes alumina abrasive grits that have a particularly’ fine mierostucture ala viteous boad mati in ‘which the alumina abrasive grits ar distribute. [0012] Taming first 0 a description ofthe alumina abrasive arts, typically the alumina abrasive grits are principally ormed of polycrystalline cealumina, The polyerystalline ‘calumina generally forms the majority phase ofthe sits, that sat least 50% by weight. Hawever, generally the al ‘mina abeasve grits are at least 60 wt. %, oftentimes at least 80 ‘wt %, and in certain embodiments at least 90 wt. % poly- enystalline c-alumina. The polyerystalline a-alumins has Tine erytalline mierosirucure that may be characterized by an aalumina average domain size not greater than S00 um. ‘The erystaline domains are discrete ideatifiable erytalline regions of the microstructure that are formed of an agarega- tion of single erystals, or may be formed ofa single erystal. However, according to certain embodiments, the erytalline domains are monocrystalline andar easily observed tough scanning electron microscopy analysis. The erystalline domain size may be even fines, such a not greater than 400 ‘im, or not greater than 300 nm. With the even finer erystal domain size, typically the domains are single erystalline as ‘noted above. Stch fine domains may be particularly small, stich as not greater than 200/nm, aot greater than 190 nem, oF {even not greater than 180 nm. Its notewony thatthe fine enystalline domain size is present in the high temperature ‘bonded abrasive component, postprocessing. Thisispariew- larly noteworthy, as ofientimes the process for Forming the high temperature bonded abrasive involves high temperature iwatment at which the vitreous bond matrix cures. Sich high temperature treatment has a tendency t0 cate domain growth, which is particularly undesirable. Further detils are provid elo: 0013] As noted above, the alumina abrasive grits further include pinning agent. pinning agent isa material that is US 2008/0148653 Al ‘oreign tothe a-aluminss microstricture ofthe grits, and ea be identified by a second phase dispersed in the polyenystal- line a-alumins matrix phase. The pinning agent is generally ‘effective to “pin” the domains, thereby preventing exagger- ‘ated domain growth during sintering andor high temperature processing of the prits to form the bonded abrasive compo- nent. Examples of a pinning agent include oxides, carbides nitrides and borides, as well as reaetion products thereof with thepolyerystalline alumina matzix. According wo parcular ‘embodiments, the pinning agent comprises an oxide of at Jeast one of silicon, boroa, tanium, zirconium, and a rare- ‘earth element, and reaction products thereof with the poly ‘eqstalline cealumina matrix. A particular pinning agent is ‘rconium oxide, generally in the form of ZrO, (zirconia). Zirconium oxide is particularly suitable material, and gener- allyis inert within te polycrystalline -alumina mate, s0as to undergo very limited reation with the alumina thereby retaining a zirconium oxide crystal phase, typically zirconia ‘Thepinning agent is generally prescat in the alumina abrasive ‘fis in an amount not less than about 0.1 w. %, such as an amount not less than about 0.5 wt. %, oF not less than about 1.Owt, %, The lower limit ofthe pinning agent is chosen to be an amount that is effective to prevent exaggerated! domain row {0014} According to one embodiment, the pinning agent is present in the abrasive grit in an amount not preser than 40 14%, suel. as am amount not greater than 30 wt. %, not nvater than 20 wt. % or even not greater than 10 wt. %. Inthe high temperature bonded abrasive, the pinning agent is gen- ‘erally identified as having a particulate size not greater than S microns, seh as aot greater than | micron, Fine particulate sizes associated with the pinning agent have been found to be useful such as aot greater than S00 am, or not greater than 300 nm, or not greater than 200 nm. As deseribed in more detail below, in the context of methods for forming high temperature bonded abrasive components, the pinning agent ‘may be intzoduced into the alumina abrasive gris ia solid orm, such as in sub-micron form, particularly including col- Joidal form. Alternatively, the pinning agent may be intro- ‘duced into the alumina abrasive grits oF precursor thereo such that upon high temperature heat twatment the pinning ‘agen precursor converts into a desired crystalline phase sch asthe desired oxide, carbide, nitride or boride [0015] Processing o form high temperature bonded abea- sive according to embodiments ofthe present invention gen- ‘erally begins withthe Formation ofthe alumi abrasive ris ‘According to particular embodiment, the alumina abrasive _ritsare formed through ascodedl proces, in which an appro= priate seding material is combines with an c-alumina pre- ‘cursor, followed by heat treatment fo convert the alumina precursor into the desired c-alumina phase. The seedsmay be Tormed in accordance with U.S, Pat No. 4,623,364, in which coded gel alumina dried precursor is calcined o form c-ali- ming. The calcined c-alumina may be further processed such asby milling to provide an appropriate high-surface area seed material. Typically the surface are is quantified by specific surface area (SSA), not less than 10 mig typically not less than 20m/g, suchas not less than 30s", oF not Tess than 40 Panicular embodiments have a surface area not less than 50 m/g, Generally, the surface area is limited, such as not greater than 300 mp, such as not greater than 250 mfg. Jun. 26, 2008 {0016} The seed materials then combined with the she ‘mina procure, which may take on anyone of several ors of alminous terials tht is an appropriate form for con- version 1 cealumina, Such prccurce materials inlode for example, hydrated aluminss, including alumina wiydeate (ATH) and boohmite. As usd herein, bochnite denotes aie sina Iydrates inching sineral bochaite, typically being AI,Oy H,0 and having a water content onthe order of 15% as well as pseudo-bochmite, having water content greater than 18%, suc as 209610 38%. As auch the tem boehiit willbe used t denote alumina hydrates having 15 10 38% wate comtent, suchas 15 to 30% water content by weight It js noted that bochmite, inching pseudo-boehmite, has a paticularand identifiable erystalstictre and accontingly a ‘nique X-ray action patter, and as sch, is distinguished from olher aluminous materials, including ether hydrated alominas {0017} ‘Typically, the a-aumina precursor, such as boeh- ites combined with th sod ansterialsuch that the seeds fre presen in an mount aot es than 0.2 wt with respect {0 tal solids content of seeds and qcaluminn precursor Typically, the seas are present in aout less han 30 wt °%.or. typically, nan aroun not greater than 20 wt 9% {0018} "Theseedsndthe calunina peecurorare generally combined in sly form which thea gle, such bythe fddtion of an appropriate acd or hase seh a aie acid Following gelation, the gels typically dried, crashed, and hicd material is posse though classification sieves. The elastied soid ation may then be subjected to sintering process that has imited soak time. Typically, sintering is famed our fra time period not exceeding, 30 minutes, such ‘snot greater than 20 minutes, not gretee than 15 mines According to particular embodiments the sintering period i particularly shor, suc as not rete than 10 minutes {0019} According o a particuar development, pining ‘gent oe pining agent pescsoe is ade tothe sispension containing seeds and alumina recurso. Type the pin- geal rFting age recs is present in. au ot greater than 40 wt % based upon the combined solids content of he c-alumisa pressor, seeds, ad pining agent rim agent prursorcalulted bas upon sols con- tent ofthe pinning agent in he final ealumina rit). Gener ally thepiingagents preset ina amount ot shan ‘wt 9%, such as not Tess than about 05 wt % or even not ss than about 1 wt. %, based upon the total Solids content as noted above {0020} Sil func, seconding to a particular development Sintering searied outta temperature above the emperatire that is necessary to effect conversion of the alumina pre cursor into cealumina, Ina sense, certain embodiments eal for “oveesntring” the alumina procrsor mister. Pat ticularly suitable temperatures are generally not less than 1380° C, sch ak not es than 1378" C., not less than 1385° mot less than 198°C. or aot less than 1400” C. In this respect, it noted that while ne microsritured seeded Ccalimina materials have boca formed in the atypically such materials are processed at lower temperatures, ofen- times below 1380" C:, such as on the onder of 1300" C Further observations on the combined eect of utilization of a pining agen andoversnteringare provided herein below. US 2008/0148653 Al 10021] Following sintering, optionally classified abrasive _ritsare then combined witha vitreous bond material, shaped Jno.an appropriate geometric eontour (eg. grinding whe), which contoursand shapes ae well appreciated inthe context ‘of the bonded abrasives at. Processing 10 complete the bonded abrasive component typically involves heat treatment at a cure temperature. As used herein, cure temperature ‘denotes a material parameter associated with the vitreous bond matrix material andi generally in excess ofthe melting temperature, and particularly, the glass transition temperature “Tofthe bonding material The eure temperature isthe mii lun temperature at which the bond matrix material not oaly softens and becomes flowable, but also becomes flowable 10 fn extent ensuring complete wetting and honing to the abra- sive gris. Typically, the cure temperature aevording 10 ubodliments herein isnot ess haa 1000° C, generally indi ‘cating formation ofa high temperature bonded abrasive 10022] Particular examples were made according to the following description. EXAMPLES Example 1 Comparative 10023] In 400 mil pyrex beaker, 30 grams of aluminum ‘oxide hydroxide (pseudo boehiite) powder under the trade name DISPERAL obtained from Sasol Ine of Hamburg Ger ‘many was sired into 61 milliliters of deionized water (ress- tivity 2 mega-ohm em), 10024] Asa seed feedstock, seeded gel alumina dried pre- ‘cursor as propre in US, Pa. No, 4,623,364 was calcined at 1100 for$ minutes ina rotary kiln to convert the alumina to form with asurfacearea as measured by the BET method of 15 to 28 m’/g. 72 kg ofthis cvaluinina feedstock was mixed “with 150kgof deionized water and fed ito horizontal bead, mill manufactured by Netz Company (headquarters Selb ‘Germany The model ofthe device was LMZ-25. Milling was conducted for 24 hours with the slurry continuously

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