USOO782.0068B2

(12) UnitedO States Patent (10) Patent No.: US 7820,068 B2 Wang et al. (45) Date of Patent: Oct. 26, 2010

(54) CHEMICAL ASSISTED LAPPING AND 6,236,542 B1 5/2001 Hartog et al. POLISHING OF METALS 6,416,685 B1 7/2002 Zhang et al. 6.569,215 B2 * 5/2003 Miyata ...... 5 1/307 (75) Inventors: Qi Wang, Birdsboro, PA (US); Donald 5: R S. Asia et al. L. Schuster, Springfield, OH (US) 6,838,149- 4 B2 1/2005 LuggCa. et al. (73) Assignee: Houghton Technical Corp., 7,005,080 B2 2/2006 Holland et al. Wilmi DE (US 7,029,373 B2 4/2006 Ma et al. ilmington, DE (US) 2001/0030152 A1 10/2001 Wright et al. - 2004/0134873 A1 7, 2004 Yao et al. (*) Notice: Subject to any disclaimer, the term of this 2005, OO14597 A1 1/2005 Michaud et al. patent is extended or adjusted under 35 2005, 0037936 A1 2/2005 Martyak et al. U.S.C. 154(b) by 147 days. 2005, 016461.0 A1 7/2005 Michaud et al. 2006/0111018 A1 5/2006 Kopp et al. (21) Appl. No.: 12/034,092 2006, O131275 A1 6, 2006 Bian et al. 2006, O151071 A1 7/2006 Bedard et al. (22) Filed: Feb. 20, 2008 2006, O185184 A1 8, 2006 McGlasson et al. (65) Prior Publication Data FOREIGN PATENT DOCUMENTS US 2008/0197112 A1 Aug. 21, 2008 WO WO 2005076871 A2 *ck 8, 2005 OTHER PUBLICATIONS Related U.S. Application Data Linetal, Effects ofSlurry Components on the Surface Characteristics (60) Provisional application No. 60/890,957, filed on Feb. when Chemcial Mechnical Polishing NiPAl Substrate, Jan. 26, 21, 2007. 2005, 483, Thin Solid Films, pp. 400-406.* Marinescu, "Loose Abrasive Processes'. Tribology of Abrasive (51) Int. C. Machining Processes, Chapter 13:500-530, Noyes, (2004). C09K I3/00 (2006.01) Howes, “Manufacturing Technology Research Needs of the Gear

(52) U.S. Cl 252/79.1 Industry'. A Manufacturing Technology Information Analysis Cen ir grgrrr. ter Report, (Dec. 31, 1987). (58) Field of Classification Search ...... None Subramanian, “Finishing Methods'. Surface Engineering, ASM See application file for complete search history. Handbook, 5:79-164, ASM International, Materials Park, OH, (1994). (56) References Cited Sroka, “Superfinishing Gears: The State of the Art, Part II”, Gear U.S. PATENT DOCUMENTS Technology, 30-32 (Jul/Aug. 2005). Baypure (R) DS 100 Solid G. Product Information Sheet, (Jul. 2004). 3,071.456 A 1, 1963 Cheesman et al. MicroSurfaceTM 5130 Product Data Sheet (Nov. 18, 2003). 3,531.414 A 9/1970 Keary et al...... 422,8 MicroSurfaceTM 5130 Material Safety Data Sheet (Nov. 2003). 3,715,842 A 2, 1973 Tredinnicket al...... 451.36 MicroSurfaceTM 5132 Product Data Sheet (Nov. 2003). 3,979,858 A 9, 1976 Semones et al. MicroSurfaceTM 5132 Material Safety Data Sheet (Nov. 2003). 4,038,048 A 7, 1977 Thrower et al. MicroSurfaceTM 5142 Product Data Sheet (Aug. 2007). 4,046,524 A 9, 1977 Van Hesden et al. MicroSurfaceTM 5142 Material Safety Data Sheet (Sep. 7, 2006). 4,181,540 A 1, 1980 Ahlfetal. MicroSurfaceTM3305-15 Material Safety Data Sheet (Sep. 8, 2006). 4,491,500 A 1, 1985 Michaud et al. 4,705,594. A 1 1/1987 Zobbietal. * cited by examiner 4,770,672 A 9, 1988 Menard et al. 4,818,333. A 4, 1989 Michaud et al. Primary to sh Tran lai 4,906,327 A 3, 1990 Michaud et al. Assistant Examiner Step anie Duclair 5,051,141 A 9, 1991 Michaud et al. (74) Attorney, Agent, or Firin—Howson & Howson LLP 5,158,623 A 10, 1992 Michaud et al. 5,158,629 A 10/1992 Zobbietal. (57) ABSTRACT RE34,272 E 6, 1993 Michaud et al. 5,299,390 A 4, 1994 Kato et al. Compositions for lapping gears and methods for preparing 5,503,481 A 4, 1996 Hashimoto et al. the same are described. These compositions contain a salt of 5,538,462 A ck 7, 1996 Gnadt et al. polyaspartic acid and may contain additional components 5,855,633. A 1/1999 Simandlet al...... 51,308 that are useful for lapping gears. Also provided are processes 5,873,770 A 2f1999 Hashimoto et al. for using the compositions described herein 6,120,355 A 9, 2000 Stadtfeld et al. 6,217,415 B1 4/2001 Ajayi et al. 6,217,421 B1 4/2001 McGlasson et al. 11 Claims, No Drawings US 7,820,068 B2 1. 2 CHEMICAL ASSISTED LAPPING AND grits provide the action force of abrading under pressure and POLISHING OF METALS the liquid carrier provides a vehicle that suspends the abra sives and lubricates or cushions the interface to minimize CROSS-REFERENCE TO RELATED metal to metal contact, reducing potential Surface damage and APPLICATIONS heat formation. Typically, machines using traditional lapping compounds must be operated under high pressures for opti This application claims the benefit of the priority of U.S. mal production efficiency. However, under Such conditions, Provisional Patent Application No. 60/890,957, filed Feb. 21, the cutting edges of the grains and grits are worn out easily, 2007. rendering frequent change over of lapping compound for 10 disposal. BACKGROUND OF THE INVENTION Historically, oil-based carriers are used in the formulations for the lapping compounds. Suitable liquids include kero This application is related to metallic Surface finishing and, sene, diesel fuel, mineral oil, Seal oil, spindle oil, and Veg specifically, to chemical assisted lapping and polishing of etable oil. In certain cases, heavy oils, greases and animal fats metallic Surface, e.g., gears, using aqueous based carriers. 15 may also be used in the composition of the carrier. To improve Lapping and polishing are widely used precision finishing the oil based carrier, a variety of oil soluble chemicals may be processes for many objects made of a variety of materials added. For example, U.S. Pat. Nos. 4,046,524 and 4,770,672 including glass, ceramic, plastic, semiconductor metals, met refer to oil-based lapping compositions. Use of an oil based als and their alloys (Loose Abrasive Processes, Chapter 13, in carrier as a vehicle for lapping operations Suffers from several Tribology of Abrasive Machining Processes by I. D. Mari shortcomings including the need for heavy cleaning of pro nescu et al. Noyes, 2004). The objects suitable for the two cessed parts, expensive waste disposal of used lapping com processes are also diverse in terms of their sizes, shapes, and pound, and potential slip and fall hazard for lapping opera functions. tors. In addition, the ever-increasing crude price also makes Gears are fundamental and essential components of trans the oil based lapping process less competitive. mission equipment, which are used for construction of both 25 Water based lapping compounds have also been proposed military and civilian machinery. Most high performance in the art. See, for example, U.S. Pat. Nos. 4,038.048 and gears today are still made with steel and are manufactured by 5,855,633 in which the aqueous carrier, like oil based carrier, first machining the steel into a blank followed by cutting to strictly serves as a vehicle to Suspend loose abrasives and form teeth. The rough gears are then heat treated and finished provide certain degrees of lubricity. with varying methods depending on requirement of the gear 30 specifications. Surface Smoothness is an important parameter Chemical assisted mechanical finishing has long been in evaluating gear performance. Generally speaking, the known and gained wide acceptance in the semiconductor finely finished gear teeth could reduce the amount of friction industry. Chemical mechanical planarization (CMP) is now between the contact Surfaces, minimize pitting, scuffing, and an integrated process in semiconductor chip manufacturing wear, thus prolonging working life of gears. In addition, it 35 and continues to be a Subject of active research, seeking also reduces the harmonic noise when gears are in use. improvement on all aspects of the technology. See, US Patent Improvement in gear manufacturing technology has always Application Publication Nos. US-2006/0131275, US-2005/ been an interest for many parties (Manufacturing Technology 0037936, and US-2004/0134873 and U.S. Pat. Nos. 7,029, Research Needs of the Gear Industry, A Manufacturing Tech 373, 6,838,149, 6,569,350, 6,416,685, and 6,236,542. The nology Information Analysis Center Report by M. A. H. 40 technology usually uses strong and aggressive chemicals to Howes, December 1987). help remove unwanted metals on the chip Surface. The com U.S. Pat. No. 6,732.606 discusses that an optimally fin mon chemicals used by these processes include hydrofluoric, ished gear should have a Surface roughness between approxi hydrochloric, nitric acids, hydrogen peroxide and other oxi mately 5 micro-inches Ra to 10 micro-inches Ra. The reduced dants. Due to the aggressive nature of the chemicals, Sophis Surface roughness, when located at the gear teeth, can reduce 45 ticated process control is incorporated in the technology to the maximum contact stress by more than fifty percent. The avoid over-finishing. Subsurface shear stress can be reduced by approximately In the metalworking industry, chemical assisted finishing thirty percent. Various finishing methods to achieve the stated also utilizes strong acids for metal Surface finishing, which Ra are provided, including examples such as electrochemical tends to etch pits and scratches deeper on the processed metal polishing and physicochemical polishing. 50 parts, making the process difficult to control, even though Even though many methods are available for gear finishing processes using mild acids such as in U.S. Pat. No. 3,979,858 (Finishing Methods, in Surface Engineering, ASM Hand might alleviate the problem to certain degrees. Overall, care book, Vol. 5, page 79-164, ASM International, Materials ful process control is required. Park, Ohio, 1994), lapping is by far the most well established To avoid the potential problem, U.S. Pat. No. 3,071.456 process for finishing the tooth surfaces of a pair of gears, 55 refers to the use of “surface conversion agents, which form a which are used in mesh with each other, especially for bevel friable layer on metal surface, with the metal removal on the gears. During lapping, loose abrasive slurry, referred as lap Surface being not only accelerated, but also selective, avoid ping compound, is introduced to the meshing tooth Surface of ing the phenomenon of deepening pits and Scratches on the two gears under load conditions, usually through nozzles near metal Surface normally associated with conventional acid the meshing point of the teeth. The process is usually involved 60 system. The 'Surface conversion agents' include various using specialized and expensive lapping machinery. U.S. Pat. phosphoric acids and their salts, nitro compounds, organic Nos. 6,217,421, 6,120,355, 5,538,462, 5,299,390 and US acids Such as citric and oxalic acids. Also discussed is barrel Patent Application Publication Nos. US-2001/0030152, finishing, a form of vibratory mass finishing, using abrasive US-2006/011 1018, and US-2006/0185184 represent recent media. However, the oxalic and phosphorus based conversion innovations in designing of the lapping equipment. 65 coatings suffer from operation inefficiency, partly due to the The lapping compound typically includes abrasive grains limited solubility of these reagents in water, especially the or grits suspended in a liquid carrier. The abrasive grains or salts of the same. US 7,820,068 B2 3 4 Still other proposals for metalworking or finishing compo Inafurther aspect, methods are provided for recycling grits sitions and processes are provided by U.S. Pat. Nos. 4,181, from used compositions. 540: 4,491.500; 4,705,594; 4,818,333; 3,071,456; 4,906,327 In yet another aspect, methods are provided for recycling (RE 34.272): 5,051,141; 5,158,623; 5,158,629; 7,005,080: used compositions. and 4,818,333 and US Patent Application Publication No. Other aspects and advantages of the invention will be US-2005/0164610. Other documents also address applica readily apparent from the following detailed description of tions of the conversion coating assisted finishing in produc the invention. tion of bearings and gears, such as U.S. Pat. Nos. 5,503,481 and 5,873,770. Chemically accelerated vibratory gear finish DETAILED DESCRIPTION OF THE INVENTION ing using high density, non-abrasive ceramic media is also 10 known. Publications related to this subject include G. Sroka In view of the deficiencies in the art discussed above, novel and L. Winkelmann titled as “Superfinishing Gears' in July/ compositions for treating metal Substrates were developed August 2005 issue of Gear Technology, pages 30-32 and US that contain salts of polyaspartic acid and aqueous carriers. Patent Application Publication No. US-2005/0014597. A These compositions are more successful in removing the related process is also discussed in U.S. Pat. No. 6,217,415. 15 Surface layers of metal Substrates. These novel compositions To Summarize, the conversion coating assisted chemical also permit the use of lower pressures during the processes of finishing process is normally practiced using vibratory mass using the compositions. Reducing the pressures slows the finishing equipment. The media used in the vibratory equip wearing of the abrasives utilized in the compositions, ulti ment could be either abrasive or non-abrasive. In practice, the mately prolonging the life of the compositions. The amount conversion coating assisted finishing processes in the art Suf of waste generated during the processes, i.e., lapping or metal fer from operation inefficiency. Generally, the processes need polishing, is reduced and the costs associated with these a minimum of several hours to achieve the desired Smooth processes are lowered. The compositions described herein ness of metal Surface, as discussed above. This time frame is provide lapping and polishing processes that run efficiently at unacceptable for lapping operations, since it involves expen reduced pressures. The compositions and processes using the sive lapping machinery and usually processes one item at a 25 same also provide easy cleaning of the processed metal Sub time. For example, commercial gear lapping only allots a few strate and processing equipment, reducing lapping and pol minutes for a pair of gears. ishing operating costs, simplifying waste disposal, and elimi There remains a need in the art for alternate and improved nating the slip and fall hazards associated with currently compositions and methods for lapping gears efficiently. utilized oil based lapping compositions. 30 In view thereof, compositions and processes for metallic SUMMARY OF THE INVENTION surface finishing are described herein. The term “metallic surface finishing', or variations thereof, as used herein refers In one aspect, a composition useful for polishing metal is to treating a metallic Surface. The processes described herein provided and contains a salt of polyaspartic acid and one or which utilize the novel compositions include chemical more chemical compounds useful for polishing a metal Sub 35 assisted lapping and polishing of metallic Surfaces. In par strate. In one embodiment, the composition contains at least ticular, chemical assisted lapping and polishing of a variety of about 9% by weight of the salt of polyaspartic acid. This metal Substrates, especially gears, is provided. composition is useful as a gear lapping composition. The term “metal substrate' or “metallic substrate', or In another aspect, a composition useful for polishing metal variations thereof, as used herein includes any metal Substrate contains a salt of polyaspartic acid, a grit; and one or more 40 that contains one or more of a metal, as understood to those chemical compounds useful for polishing a metal Substrate. skilled in the art. In one embodiment, the metal substrate In a further aspect, a composition useful for polishing includes one metal or a combination of metals, i.e., metal metal, e.g., gear lapping, contains water, at least 9% by weight alloys. In another embodiment, the metal includes iron, man of a sodium salt of polyaspartic acid, Sodium 3-nitrobenze ganese, copper, aluminum, chromium, cobalt, molybdenum, nesulfonate, citric acid, sodium tripolyphosphate, anhydrous 45 nickel, titanium, tungsten, Vanadium, Zirconium, magnesium, monosodium phosphate, disodium dihydrogen pyrophos among others, and alloys thereof. The metal Substrate may phate, and sodium carboxymethyl cellulose. contain one or more additional non-metallic components In still another aspect, such a composition contains water, including carbon, silicon, Sulfur, phosphorus, among others. the sodium salt of polyaspartic acid, sodium 3-nitrobenzene The compositions described herein are especially useful for Sulfonate, citric acid, sodium tripolyphosphate, anhydrous 50 coating metal Substrates that contain iron, including iron monosodium phosphate, disodium dihydrogen pyrophos alloys. In one embodiment, the compositions provided herein phate, a grit, and Sodium carboxymethyl cellulose. are useful for treating steel. In yet a further aspect, processes for polishing metal Sur faces are provided and include polishing a metal Substrate A. Lapping and Polishing Compound Composition and Surface using one or more compositions described herein. 55 Preparation Thereof In another aspect, processes for lapping gears are provided The compositions described herein are therefore useful for and include lapping gears using one or more compositions treating metal Substrates and contain one or more of a carrier, described herein. an active chemical capable of reacting with a metal Substrate, In still a further aspect, processes for preparing one or more and a salt of polyaspartic acid. In one aspect, the compositions of the compositions described herein are provided and 60 provided herein contain a salt of polyaspartic acid, one or include mixing the components of said composition using a more chemical compounds useful for polishing a metal Sub pump at room temperature. strate, i.e., “active chemicals', and, optionally, a grit. In yet another aspect, a product is provided and includes Among useful salts of polyaspartic acid for inclusion in the one container containing at least about 3% by weight of a salt compositions described herein are water-soluble salts of pol of polyaspartic acid and one or more chemical compounds 65 yaspartic acid. In one embodiment, the salt is an alkali metal, useful for finishing a metal Substrate and a second container amine, ammonium or phosphonium salt of polyaspartic acid. containing a grit. Desirably, the alkali metal salt of polyaspartic acid includes US 7,820,068 B2 5 6 the lithium, potassium and Sodium salt of polyaspartic acid. particle size includes grits of a diameter of at least 0.1, 0.5, 1. In one embodiment, the salt is the sodium salt of polyaspartic 10, 20, 30, 40, 50, 60, 70, 80, 90 and 100 um, including acid. The Sodium salt of polyaspartic acid has several pur integers and fractional diameters therebetween. In one poses in the compositions provided herein. In one aspect, the example, the average particle size of the grit is about 20 to Sodium salt of polyaspartic acid acts as a metal chelating about 25 um in diameter. In another example, the average agent. In another aspect, the sodium salt of polyaspartic acid particle size of the grit is about 4 to about 50 um in diameter. acts as a Surfactant. In yet a further aspect, the Sodium salt of In a further example, the average particle size of the grit is polyaspartic acid acts as an accelerator. about 10 to about 40 um in diameter. However, coarse par In one embodiment, the composition contains at least about ticles, i.e., larger than 5 um particles in diameter, may be 0.1 to about 15% of the sodium salt of polyaspartic acid. In 10 desired for easy recycling of the spent compositions. The another embodiment, the composition contains at least about particles of the loose grains and grits may also be irregularly 3% by weight of the sodium salt of polyaspartic acid. In one shaped, may contain sharp edges, may be spherical, or may be example, the composition contains up to about 15% of the spherical without much cutting action. Typically, the loose Sodium salt of polyaspartic acid. In a further example, the grains and grits are present in the composition up to about composition contains about 0.01 to about 12% by weight of 15 95% by weight of the final composition. In one embodiment, the Sodium salt of polyaspartic acid. In another example, the the loose grains and grits are present in the composition at composition contains about 3% to about 15% by weight of the about 25% up to about 95% by weight of the final composi Sodium salt of polyaspartic acid. In a further example, the tion. The percentage by weight of the grits in the composi composition contains about 9% to 15% by weight of the tions therefore include at least about 25,35, 45,55, 65, 75, 85 Sodium salt of polyaspartic acid. In another example, the and 95%, including integers and fractional percentages ther composition contains about 9.5% to about 15% by weight of ebetween. In one example, the loose grains and grits are the sodium salt of polyaspartic acid. In still a further example, present in the composition at about 25 to 75% by weight. In the composition contains about 9.7 to about 15% by weight of one example, the loose grains and grits are present the com the salt of polyaspartic acid. Thus, for example, the compo position at about 68% by weight. sition can contain in percentages by weight at least about 0.1. 25 The composition described herein desirably contains a car 0.5, 1,2,3,4,5,6,7,8,9, 10, 11, 12, 13, or 14 to at least about rier. In one example, the carrier is an aqueous carrier. In one 15%, and fractional percentages by weight therebetween of embodiment, the carrier is included in the composition, the Sodium salt of polyaspartic acid. thereby permitting use of the product by the customer without In one embodiment, the composition contains loose grains addition of further carrier. In another embodiment, the carrier and grits. The terms “grits”, “grains”, “loose grains”, “loose 30 is present in the composition in Sufficient amounts to provide grits', and “loose grains and grits' may be used interchange a stable solution for further dilution by the customer prior to ably and include inorganic and organic materials that may be use. In another embodiment, the carrier is added by the cus utilized to treat a metal Substrate Surface, including metal tomer to a concentrated composition prior to use. In one polishing. The loose grains and grits are prepared from a embodiment, the carrier includes water. In one example, the variety of inorganic and organic materials known to the 35 composition contains about 10 to about 30% by weight water. skilled artisan. The inorganic materials include, but are not In another example, the composition contains about 30% by limited to, diamond, cubic boron nitride, silicon carbide, alu weight water. In another example, the composition contains minum oxide, 38 white aluminum oxide corundum, garnet, about 24% by weight. However, more water may be added to quartz, glass, alumina, chromium oxide, silica oxide, carbo the composition to ensure that the final composition contains rundum, emery, ceramic, titanium oxide, manganese oxide, 40 sufficient water for use by the customer. Typically, the final Zirconium oxides, hafnium oxides, tungsten oxides, vana composition utilized for the metal polishing or gear lapping dium oxides, niobium oxides, tantalum oxide, molybdenum contains about 85% by weight water. Thus, a composition as oxides, and other Suitable metal oxides and their mixtures. described herein may contain carrier in a percentage by Organic materials for these grits include, without limitation, weight of at least 10, 20, 30, 40, 50, 60, 70, 85, up to about various homo and co-polymers, preferably with polymers 45 85%, including integers and fractional percentages therebe having certain degrees of cross-linking either via covalent or tWeen. ionic bonds. The polymers include, but are not limited to, The composition may also include one or more of an active polyvinyl chloride and other chlorinated polymers, Teflon R chemical. The term “active chemical as used herein refers to polymer and related fluoropolymers, polymethacrylate, poly a chemical compound that is capable of interacting, e.g., acrylate, polyethylene, polypropylene, polybutylene, poly 50 reacting, with a metal Substrate Surface. The active chemical styrene, polyvinylacetate, polyesters, polyamides, polyim is desirably capable of removing layers of metal atoms from ides, polysiloxanes, polyethers, polyamines, polythioethers, a metal Substrate. Thus, a composition as described herein polylactones, polylactamides, polycarbonate, and their co may contain an active chemical in a percentage by weight of polymers and cross-linked polymers. Both synthetic and at least 3, 5, 10, 15, 20, 25, 30 and up to about 35%, including natural rubbers, either modified or unmodified are possible 55 integers and fractional percentages therebetween. Desirably, organic materials. Further, polymers with a core shell struc the active chemicals are present in the composition at up to ture are also preferred and the polymers may be functional about 45% by weight. In one example, the remaining com ized with a variety of functional groups such as acidic group. ponents of the composition are present at about 3 to about Examples in this category include the Nafion R. H reagent and 35% by weight. the acid form of the Amberlyst(R) reagent, the sulfonated divi 60 In one embodiment, the active chemical is an acid and/or a nylbenzene/styrene polymer. Composite materials made with salt of that acid in monomeric, oligomeric, and/or polymeric both inorganic chemicals and organic polymers are also forms, or combinations thereof. In one example, the active included. In one example, the loose grains and grit include chemical is a strong inorganic acid including, without limi Zirconium oxides, aluminum oxides, hafnium oxides, and tation, hydrofluoric, hydrochloric, nitric, Sulfuric, Sulfamic, combinations thereof. 65 hexafluorophosphoric, hexafluorosilicic, hexafluorozirconic, The average particle size of the loose grains and grits useful hexafluorotitanic, fluorosulfonic, tetrafluoroboric, phospho herein are about 0.1 um to about 100 um in diameter. This ric, pyrophosphoric, tripolyphosphoric, metaphosphoric, US 7,820,068 B2 7 8 orthophosphoric, polyphosphoric, or thiophosphoric acid. In Sodium, potassium, and ammonium fluorides, thiocyanates, another example, the active chemical is a salt of an acid polyphosphates, and the Sodium salt of polyaspartic acid. In including, but not limited to, ammonium hydrogen difluoride, another embodiment, the metal chelating agent is the Sodium ammonium fluoride, ammonium hexafluorosilicate, ammo salt of polyaspartic acid. nium hexafluorozirconate, ammonium hexafluorotitanate, In still a further embodiment, the active chemical includes phosphate salts such as ammonium phosphate, ammonium an organic acid. In one example, the active chemical includes pyrophosphate, ammonium polyphosphate, ammonium a strong organic acid including, but not limited to, methane hexafluorophosphate, potassium hexafluorophosphate, sulfonic, benzenesulfonic, toluenesulfonic, trifluo potassium phosphate, potassium pyrophosphate, potassium romethanesulfonic, trifluoroacetic, phytic, glycerophospho polyphosphate, sodium hexafluorophosphate, sodium poly 10 ric, 2-ethylhexyl phosphoric, butylphosphonic acids and phosphate, sodium phosphate, or Sodium pyrophosphate, ammonium, potassium, and Sodium salts of these acids. In potassium hydrogen difluoride, potassium fluoride, potas another embodiment, the active chemical includes weak sium hexafluorosilicate, potassium hexafluorozirconate, organic acids including, but not limited to, formic, acetic, and potassium hexafluorotitanate, sodium hydrogen difluoride, other C to Cs carboxylic acids in straight or branched chains Sodium fluoride, Sodium hexafluorosilicate, sodium 15 optionally functionalized with hydroxyl, carbonyl, thiocar hexafluorozirconate, sodium hexafluorotitanate; zinc, man bonyl, mercapto, amino, and other functional groups. ganese, ferrous, and ferric salts thereof, and phosphorus and Examples of C to Cs carboxylic acids useful in the compo thiophosphorus acids. In a further example, the composition sition contain glycolic, thioglycolic, lactic, gluconic, and a contains one or more of a phosphate salt. In yet another variety of amino acids, either synthetic or natural. Di, tri, and example, the composition contains sodium tripolyphosphate, tetra-carboxylic acids and their anhydrides such as oxalic, anhydrous monosodium phosphate, disodium dihydrogen malonic, succinic, malic, thiomalic, tartaric, maleic, glutaric, pyrophosphate, or any combination thereof. When the com adipic, citric, oligomeric and polymeric carboxylic acids position contains one or more of a phosphate salt, the total based on C to C monomers such as polyacrylic, poly phosphate salts is up to about 15% by weight of the compo methacrylic, polyaspartic, polyglutamic, and other polyami sition. Thus, for example, the composition may contain in 25 nodicarboxylic acids, as well as their salts are also examples percentages by weight of at least 0.01, 0.05, 0.1, 0.5, 1, 2, 3, of active chemicals that may be included in the compositions. 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, or 14 to at least about 15%, and Desirably, one active chemical in the composition is Oxalic fractional percentages by weight therebetween of the phos acid. The salts of ammonium, Sodium, potassium, zinc, mag phate salt. In another example, the composition contains nesium, ferrous, ferric, quaternary ammonium, phospho about 0.01 to about 15% by weight of phosphate salts. In a 30 nium, and Small water-soluble organic amines are further further example, the composition contains about 0.01 to included for these weak organic acids. In one example, the about 10% by weight of phosphate salts. In another example, composition contains citric acid. Desirably, the acid is present the composition contains up to about 5% by weight of each in the composition at up to about 15% by weight. Thus, for phosphate salt. In yet another example, the composition con example, the composition may contain percentages by weight tains about 0.01 to about 5% by weight of each phosphate salt. 35 of at least about 0.1, 0.5, 1,2,3,4,5,6,7,8,9, 10, 11, 12, 13, In a further example, the composition contains about 0.01 to or 14 to at least about 15%, and fractional percentages by about 3% by weight of each phosphate salt. In another weight therebetween, of the acid. In one example, the com example, the composition contains about 2.4% by weight of position contains about 0.1 to 10% by weight of the acid. In each phosphate salt. In still a further example, the composi another example, the composition contains about 1.6% by tion contains Sodium tripolyphosphate at about 1.2% by 40 weight of the acid. weight. In yet another example, the composition contains In yet a further embodiment, the active chemical may anhydrous monosodium phosphate at about 0.1% by weight. include dichromates, molybdates, Zirconates, manganates, In still a further example, the composition contains disodium and other metal based oxo compounds, either in higher or dihydrogen pyrophosphate at about 1% by weight. lower Valent states. High Valence halogen compounds such as In another embodiment, the active chemical includes a 45 perchlorate and periodate may also be used as the active metal chelating agent. The term “metal chelating agent’ as chemical. In one example, the active chemical is sodium used herein refers to a chemical compound that binds to a dichromate, potassium dichromate, sodium molybdate, metal substrate. Desirably, the composition described herein potassium molybdate, Sodium Zirconate, and potassium Zir includes a salt of a polyamino acid, Such as polyaspartic acid. COnate. In one embodiment, the salt of polyaspartic acid is the Sodium 50 In still a further embodiment, the active chemical may salt of polyaspartic acid. Additional metal chelating agents include oxidizing agents including, without limitation, may be included in the composition and include, without hydrogen peroxide, inorganic peroxides Such as percarbo limitation, fluorides, ammonia, Sodium and Sodium thiocyan bates, perborates, persulfate, or perphosphates, or organic ate, di and polyamines, EDTA, polyphosphates, aminocar hydroperoxides and peracids such as t-butyl hydroperoxide, boxylic acids and their polymers, 1,3-diketones, hydroxycar 55 cumene hydroperoxide, 2-methyl-2-hydroperoxy-5-hy boxylic acids, phosphonic acids, oximes, Schiffbases, crown droxy-pentane, peracetic acid, or perbenzoic acid. Various in ethers, polyethers, poly and cyclic Sulfur compounds, poly situ generated peroxy compounds may also be included in the acrylate, polymethacrylate, polymethacryloyl acetate, poly composition, which are stabilized by chemical compounds, vinyliminodiacetic acid, polyvinylpyrrolidone and its including those discussed in U.S. Pat. Nos. 4,636,368, 4,064. copolymers, polyamines, and other polymers such as poly(p- 60 064, 4,059,678, 4.203,765 and 4,557,935, which are hereby vinylbenzyliminodiacetic acid) and polymethacryloylac incorporated by reference. In one example, the composition etone. Additional metal chelating agents may be selected by includes hydrogen peroxide. one skilled in the art for use in the compositions described In yet another embodiment, the active chemical contains herein and include those provided in Chelating agents, in one or more of an accelerator. The term “accelerator” as used Kirk-Othmer Encyclopedia of Chemical Technology, 4" Edi 65 herein refers to a chemical compound that speeds up a chemi tion, Volume 5, page 764, which is hereby incorporated by cal reaction with a metal Substrate Surface. A variety of accel reference. In one embodiment, the metal chelating agent is erators are useful in the composition. In one example, the US 7,820,068 B2 9 10 accelerator is nitro and nitroso containing compounds, both isothiazolin-3-ones, glutaraldehyde, quaternary ammonium organic and inorganic, including, but is not limited to, sodium and phosphonium salts, including the biocides described in nitrate, Sodium nitrite, ammonium nitrate, ammonium nitrite, catalogs such as “Industrial Biocides”, 2005 (ISP) and potassium nitrate, potassium nitrite, sodium and sodium salts “Dowicide A Antimicrobial, 1983: “Dowicil 75'., 1981; and of 2,4-dinitrobenzenesulfonic and dinitrobenzoic acids, “Dowicil QK-20 Antimicrobial, 1999 (Dow Chemical), Sodium and potassium salts of 3-nitrobenzenesulfonic acid, which are hereby incorporated by reference. dinitroanilines, naphthol yellow S, and cupferron. Hydroxy In other embodiments, an antioxidant is added to the com lamines, amine oxides, quinones, nitronium and nitrosonium position as an active chemical to prolong the useful life of the salts, and amino carboxylic acids and their polymers may also composition. The addition of the antioxidant depends on the be used as accelerators. Metallic salts including ferrous and 10 requirements of the manufacturing process and other compo ferric sulfate are also used as an accelerator in the composi nents on the formulation and can be determined by one skilled tions described herein. In one embodiment, the accelerator is in the art. Examples of useful antioxidants include phenolic Sodium nitrate, potassium nitrate, nitrite, 3-nitrobenezene based antioxidants, amine based antioxidants, or a combina Sulfonate, naphthol yellow S, and polyaspartic acid and its tion thereof. Ascorbic and citric acids, as well as non-phe Sodium salt. In another embodiment, the accelerator is 3-ni 15 nolic antioxidants as discussed in U.S. Pat. Nos. 7,053,139 trobenzenesulfonate. Typically, the accelerator is present at and 7.019,055, which are hereby incorporated by reference, up to about 5% by weight. Thus, for example, the composition are also included in the composition in certain embodiments. may contain in percentages by weight at least about 0.01, In one embodiment, the antioxidant includes phenol and 0.05, 0.1, 0.5, 1, 2, 3, or 4 to about 5% of the accelerator, and amine based antioxidants. fractional percentages by weight therebetween, of the accel In another embodiment, leveling agents or burnishing erator. In one example, the accelerator is present at about 0.01 compounds are included in the composition as an active to about 3% by weight. In another example, the accelerator is chemical(s). The addition of the leveling agent depends on the present at about 0.1% by weight. requirements of the manufacturing process and other compo Inafurther embodiment, the active chemical is a surfactant nents on the formulation and can be determined by one skilled and is added as component of the composition. The Surfactant 25 in the art. Examples of leveling agents include those utilized is particularly useful as a wetting and/or slipping agent, which in the electroplating industry and include, but are not limited use may be determined by one skilled in the art. The surfac to, 2-butene-1,4-diols, 2-butyne-1,4-diols, urea, thiourea, tant can be anionic, cationic, nonionic, or amphoteric. Useful Sodium saccarin, and organic quaternary ammonium salts. Surfactants include, but are not limited to, alkylaryl Sulfonate, The inventors found that the use of leveling agents in the fatty acid salts, alkoxylated fatty amines and alcohols, alky 30 composition improved the lapping and polishing effect of the lated amines, ether carboxylic acids and its salts, and lecithin. processed metal objects. The surfactant also includes polyhydroxy containing com In still other embodiments, a thickening agent is incorpo pounds and water soluble polymers and includes, without rated into the composition as an active chemical. The addition limitation, polyalkylene glycols including ethylene glycol, of the thickening agent depends on the process requirements propylene glycol, butylenes glycol, and hexylene glycol, 35 and the other components of the composition. The thickening Sugar alcohols, Sugar, Sugar molasses, polyvinylalcohol, Sul agent includes, without limitation, Xanthan gum, modified fonated polyvinylstyrene, poly(acrylic/styrene) copolymer, cellulose polymers, agar, modified and unmodified Starch, polyvinylpyrrolidone and its copolymers, polyacrylate, poly chitin, chitosan, other polysaccharides, partially hydrolyzed oxazolines, and salts of polyamino carboxylic acid such as the polyvinylacetate, polyvinylalcohol, polyvinylpyrrolidone Sodium salt of polyaspartic acid. In one embodiment, the 40 and its copolymers, polyacrylate, polyoxazolines, polyethers, Surfactant includes alkoxylated fatty alcohols and the sodium polyamines, aluminum salts of fatty acids, and certain min salt of polyaspartic acid. erals. In one embodiment, the thickening agent is chitosan or In still a further embodiment, the active chemical is a sodium carboxymethylcellulose. In another embodiment, the slipping agent. A number of slipping agents are available for thickening agent is sodium carboxymethylcellulose. The use in the composition and include glycerol, without limita 45 thickening agent is typically present in the composition at up tion. to about 5% by weight. Thus, for example, the composition In another embodiment, the composition includes rust pre may contain in percentages by weight at least about 0.01, ventives, which may be determined by one skilled in the art, 0.05, 0.1, 0.5, 1, 2, 3, or 4 to about 5%, and fractional per as an active chemical. Rust preventatives that are useful in the centages by weight therebetween, of the thickening agent. In compositions described herein include, but are not limited to, 50 one example, the thickening agent is present in the composi Sodium nitrite, potassium nitrite, benzoic acid, benzoic acid tion at about 0.01 to about 2% by weight. In another example, salts, dicarboxylic acids, dicarboxylic acid salts, benzotriaz the thickening agent is present in the composition at about oles, tolyltriazoles, and quaternary ammonium salts, includ 0.6% by weight. It should be understood that all integers and ing the rust preventatives marketed by Lonza and the rust fractional percentages of between 0.01 to about 2% by weight preventives provided in catalogs such as “TecGard Metal 55 are included within this range. working Additives” (Afton Chemical) and “Metalworking A pH adjustor or buffer is added as a component of certain Specialties' (PCC Chemax), which catalogs are hereby incor embodiments of the composition as an active chemical to porated by reference. In one embodiment, the rust preventive adjust pH. Examples of useful pH adjustors or buffers is sodium nitrite, salts of dicarboxylic acids, benzotriazoles, include, without limitation, Sodium hydroxide, potassium and tolyltriazoles. 60 hydroxide, ammonium hydroxide, Sodium carbonate, potas To prevent biological growth in the composition, either in sium carbonate, ammonium carbonate, Sodium bicarbonate, storage or during use thereof, biocides are optionally included potassium bicarbonate, ammonium bicarbonate and other as an active chemical. The addition of the biocide depends on basic compounds such as water-soluble amines including the requirements of the manufacturing process and other alkanolamines such as monoethanolamine or triethanola components on the formulation and can be determined by one 65 mine. In one embodiment, the pH adjustor is sodium hydrox skilled in the art. Biocides useful in the composition include, ide, sodium carbonate, or citric acid. Desirably, the pH of the but are not limited to, formaldehyde releasing chemicals, composition is about 0.5 to about 13 depending on the chemi US 7,820,068 B2 11 12 cals used in the specific formula. Thus, the pH range includes In still a further example, a first composition is provided 0.5, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, and 13 as well as and includes water, at least 9% by weight of a sodium salt of fractional pH numbers therebetween. In one embodiment, the polyaspartic acid, sodium 3-nitrobenzenesulfonate, citric pH is about 2 to about 6. acid, Sodium tripolyphosphate, anhydrous monosodium In one embodiment, the compositions described herein are phosphate, disodium dihydrogen pyrophosphate, and Sodium particularly useful in lapping steel Substrates. These compo carboxymethyl cellulose. sitions desirably contain a salt of polyaspartic acid, active In an example of a complete composition, the composition chemicals includes oxalic acid and various phosphorus based includes water, sodium salt of polyaspartic acid, Sodium 3-ni acids and their salts, as described above and which are widely trobenzenesulfonate, citric acid, Sodium tripolyphosphate, available and inexpensive. In view of the deficiencies of 10 anhydrous monosodium phosphate, disodium dihydrogen oxalic and phosphorus based conversion coatings previously pyrophosphate, a grit, and Sodium carboxymethyl cellulose. discussed, the inventors introduced organic based phospho In a further example, a composition is provided and rus acids and salts thereof and water Soluble organic amines includes about 24.4% by weight of water, about 3% by weight into the composition described herein. The introduction of the of the sodium salt of polyaspartic acid, about 1.6% by weight organic based phosphorus acids and salts thereof permitted 15 of citric acid, about 1.2% by weight of sodium tripolyphos gear lapping to be performed at commercial speeds. Further, phate, about 0.1% by weight of anhydrous monosodium the amines permitted the use of more oxalic and various pyrophosphate, about 1% by weight of disodium dihydrogen phosphorous based acids in the composition. Examples of pyrophosphate, about 68% by weight of zirconium, alumi organic based phosphorus acids and salts thereof active num, and hafnium oxides, about 0.6% by weight of sodium chemicals useful in the compositions include, but are not carboxymethylcellulose, and about 0.1% by weight of limited to, phytic, glycerophosphoric, 2-ethylhexyl phospho sodium 3-nitrobenzenesulfonate. ric, butylphosphonic acids and their salts. Examples of amine In still a further example, a composition is provided and active chemicals useful in the composition include, without includes about 10 to about 30% by weight of water, about limitation, alkanolamines such as triethanolamine. Further, 0.01% to about 12% by weight of the sodium salt of polyas the inclusion of loose grains and grits in this composition 25 partic acid, about 0.01 to about 10% by weight of citric acid, permitted the use of excess oxalic and phosphorus com about 0.01 to about 5% by weight of sodium tripolyphos pounds, beyond their normal solubility at room temperature. phate, about 0.01 to about 5% by weight of anhydrous mono The inventors found that the excess Oxalic and phosphorus sodium pyrophosphate, about 0.01 to about 5% by weight of compounds were absorbed by the loose grains and grits. The disodium dihydrogen pyrophosphate, and about 0.01 to about inventors hypothesized that the absorbed oxalic and phospho 30 2% by weight of sodium carboxymethylcellulose. rus compounds were dispersed on the Surfaces of the loose In yet another example, a composition is provided and grains and/or grits either in molecular monolayer or as nano includes about 10 to about 30% by weight of water, about 9% particles, which then permitted the direct reaction between by weight of the sodium salt of polyaspartic acid, about 0.01 the same and the metal Surface. By doing so, the compositions to about 10% by weight of citric acid, about 0.01 to about 5% permitted the lapping and polishing of metal Substrates to 35 by weight of sodium tripolyphosphate, about 0.01 to about complete in minutes instead of hours. 5% by weight of anhydrous monosodium pyrophosphate, The product can be provided to the customeras a complete about 0.01 to about 5% by weight of disodium dihydrogen neat composition, requiring dilution; as a ready for use com pyrophosphate, and about 0.01 to about 2% by weight of position, requiring no dilution; or as a two part composition in sodium carboxymethylcellulose. which the grits are provided separate from the remainder of 40 In a further example, a composition is provided and con the Solution and the customer is required to admix the grits tains about 10 to about 30% by weight of water, about 0.01 to into the other components prior to use with dilution optional. about 12% by weight of the sodium salt of polyaspartic acid, In one example, a product is provided and includes a first about 0.01 to about 10% by weight of citric acid, about 0.01 container which contains at least about 3% by weight of a salt to about 5% by weight of sodium tripolyphosphate, about of polyaspartic acid and one or more chemical compounds 45 0.01 to about 5% by weight of anhydrous monosodium pyro useful for finishing a metal Substrate. The product may also phosphate, about 0.01 to about 5% by weight of disodium contain a second container which contains one or more of a dihydrogen pyrophosphate, about 0.01 to about 2% by weight grit. Upon use, the customer mixes the grit from the second of sodium carboxymethylcellulose, about 0.01% to about 3% container into the components of the first container. by weight of sodium3-nitrobenzenesulfonate; and about 25% For example, the first container optionally contains citric 50 to about 75% by weight of zirconium, aluminum, and acid, Sodium tripolyphosphate, anhydrous monosodium hafnium oxides. pyrophosphate, disodium dihydrogen pyrophosphate, In still another example, a composition is provided and Sodium carboxymethylcellulose, sodium salt of polyaspartic contains a salt of polyaspartic acid, oxalic acid, and a grit. acid, and sodium 3-nitrobenzenesulfonate. In another This composition may further contain one or more chemical example, the first container contains about 76% by weight of 55 compounds useful for polishing a metal Substrate. water, about 9.5% by weight of the sodium salt of polyaspar The compositions described herein are typically prepared tic acid, about 5% by weight of citric acid, about 4% by by combining the components of the composition in a reactor. weight of sodium tripolyphosphate, about 0.3% by weight of One skilled in the art would readily be able to select a suitable anhydrous monosodium pyrophosphate, about 3% by weight reactor for use thereof. Desirably, the compositions are pre of disodium dihydrogen pyrophosphate, about 2% by weight 60 pared at room temperature or above. In one embodiment, the of sodium carboxymethylcellulose; and about 0.3% by composition is prepared by combining warm water and the weight of sodium 3-nitrobenzenesulfonate. other components of the composition and then adding the In a further example, a first composition is provided and loose grains and grits. By adding the grits separately to the contains a salt of polyaspartic acid, Sodium 3-nitrobenzene remainder of the composition at an elevated temperature, the Sulfonate, citric acid, sodium tripolyphosphate, anhydrous 65 inventors found that the solubility of the other components monosodium phosphate, disodium dihydrogen pyrophos was increased. In another embodiment, the composition is phate, and sodium carboxymethylcellulose. prepared at room temperature. This method includes combin US 7,820,068 B2 13 14 ing the room temperature water with the other components of the composition is fed to metal using an individual holding the composition, followed by addition of the loose grains and vessel. In a further example, the composition is added via grits. Efficient and extended agitation may be required if the nozzles through a circulation system to mesh gear Surfaces. room temperature method is utilized. Thickeners, if utilized However, the method utilized to contact the metal with the as a component of the composition, are typically added last. 5 composition is not a limitation on the present invention. In one embodiment, the compositions are prepared using a When the composition is applied to a gear, the composition pump. One skilled in the art would readily be able to deter polishes the metal using techniques known to those skilled in mine when the components of the composition have been the art of lapping gears. Various modifications may be made sufficiently combined and a uniform mixture thereofhas been by one skilled in the art. One skilled in the art would also obtained. Typically, the uniformity of the composition is 10 recognize when the metal Surface, i.e., gear, has been Suffi determined by density or visually. ciently lapped using techniques in the art. For example, one The compositions described herein may be prepared and skilled in the art would be able to examine the metal surface, provided in several forms. In one example, the composition is i.e., gear Surface, by instruments or visually to determine the prepared by combining all of the components including the Smoothness and pitting of the metal and thereby completion carrier, Sodium salt of polyaspartic acid, and one or more 15 of the process. active chemicals. This composition may then be utilized with Alternatively, the compositions described herein are useful out further modification. In another example, the composition for polishing metal Substrates using vibratory processes. is prepared by combining the Sodium salt of polyaspartic acid, Typically, compositions useful for this purpose contain loose one or more active chemicals, and the grit. Prior to use, this grains and grits. In one example, the composition is applied to composition is combined with the carrier, which may be the metal. In a further example, the metal is immersed in the separately purchased by the customer. Alternatively, the com composition. position may be present in a product in one container, whereby a second container may be present in the product and C. Method of Refortifying and Recycling the Aqueous Based separately include the carrier. In a further example, the com Lapping and Polishing Compound position is prepared by combining the Sodium salt of polyas 25 To further reduce lapping cost and increase environmental partic acid, one or more active chemicals, and the carrier. friendliness, a method is also provided for refortifying and Prior to use, this composition is combined with the grit, which recycling the compositions described herein. The inventors may be separately purchased by the customer. Alternatively, found that methods of reusing and recycling oil based lapping the composition may be present in a product in one container, compounds are economically unfeasible for a variety of rea whereby a second container may be present in the product and 30 sons. For example, the loose abrasives in the spent oil based separately include the grit. lapping compound typically lose their cutting ability. In addi In one embodiment, a product is provided and includes a tion, separation of oil from the loose abrasives in the oil-based first container containing at least about 3% by weight of a salt compositions in the art requires considerably more energy. of polyaspartic acid and one or more chemical compounds Therefore, since the most expensive component of a lapping useful for finishing a metal Substrate and a second container 35 composition tends to be the loose grains and grits, recovery of containing one or more of a grit. In one example, the first this component was advantageous. container contains about 9.5% by weight of the sodium salt of Since the composition described herein permits commer polyaspartic acid. In a further example, the first containeralso cial lapping of metal Substrates to be performed at lower contains citric acid, Sodium tripolyphosphate, anhydrous pressures, less cutting action is required from the loose grains monosodium pyrophosphate, disodium dihydrogen pyro 40 and grits at these lower pressures. Therefore, the loose grain phosphate, Sodium 3-nitrobenzenesulfonate, and Sodium car and grits have a prolonged working life and can be recycled boxymethylcellulose. In another example, the first container for reuse at a late date. contains about 76% by weight of water, about 9.5% by weight In one embodiment, the loose grains and grits are recycled of the sodium salt of polyaspartic acid, about 5% by weight of and reused by collecting the spent, i.e., used, composition and citric acid, about 4% by weight of Sodium tripolyphosphate, 45 refortifying it by adding more components of the original about 0.3% by weight of anhydrous monosodium pyrophos composition into the spent composition. The terms "spent’ or phate, about 3% by weight of disodium dihydrogen pyro “used describe a composition provided herein that has been phosphate, about 2% by weight of sodium carboxymethyl utilized to polish, treat, or lap a metal substrate surface. This cellulose; and about 0.3% by weight of sodium used/spent composition may be collected by one skilled in the 3-nitrobenzenesulfonate. 50 art and utilized as described herein. Still other compositions are able to be assembled by one In one example, the additional components are added skilled in the art given this description and the knowledge of incrementally to the holding tank during the lapping opera the art. tion. In another example, the additional components are all added at once in a centralized waste holding vessel where the B. Methods of Lapping Metal Objects Using the Aqueous 55 spent composition is lapping collected. The amount of each Based Lapping and Polishing Compound component added to the spent composition may be deter The compositions described herein can be utilized for a mined by one skilled in the art. The spent lapping composi variety of purposes and in a variety of industries. In one tion may also be diluted with water, if necessary. embodiment, the compositions are useful for polishing metal In another example, the loose grains and grits may be Substrates, and specifically, metal Surfaces, and may be uti 60 collected from the spent lapping composition. A variety of lized on any commercial lapping equipment. In another procedures known to those skilled in the art may be utilized to embodiment, the compositions are useful for lapping gears. collect the loose grains and grits and include, without limita In a further embodiment, the compositions are useful treating tion, centrifugation and filtration. The isolated loose grains metal Substrates using vibratory processes. and grits can then be further washed using clean water, if Typically, the metal is treated using the composition and 65 required. These recovered loose grains and grits may then be polished using the same. In one example, the composition is reused for preparation of new batches of the lapping and Supplied to the metal using a central tank. In another example, polishing compound. US 7,820,068 B2 15 16 In one example, a method is provided for preparing a and duration were based on the existing gear production composition for lapping gears including analyzing the com protocol using oil based lapping compounds known in the art. ponents of a used composition and adding one or more of a After the operation, the processed gears were simply rinsed salt of polyaspartic acid, water, grit, and/or active chemical to with water and mounted onto testing equipment to examine the used composition. By doing so, a composition useful for polishing metal is provided. both the lapping pattern and noise level. If necessary, the In a further example, a method is provided for preparing a described lapping procedure was repeated, and progress of composition for lapping gears including analyzing the com lapping was examined again with the testing equipment. ponents of a used composition and adding one or more of a The data showed that the compositions prepared in salt of polyaspartic acid, water, a thickening agent, accelera 10 Example 1 resulted in improved lapping pattern of the gears tor, acid, grit, and phosphate Salt to the used composition. By in comparison with the composition made from all the ingre doing so, a composition useful for polishing metal is pro dients in Example 1 except the Sodium salt of polyaspartic vided. acid. In another example, a method for recycling grits from a used composition is provided. This method includes isolating 15 the grits from the used composition. One skilled in the art Example 4 would readily be able to isolate the grits using techniques in the art including filtration, centrifugation, among others. The Preparation of a Composition Containing a Salt of isolated grits may then be washed, preferably using water. Polyaspartic Acid and Grains/Grits The following examples are illustrative only and are not intended to be a limitation on the present invention. The composition prepared as described in Example 1 was combined with Zirconium, aluminum, and hafnium oxides EXAMPLES (21.560 g) for about 4 hours using a high speed agitator to provide a uniform dense muddy material. Example 1 25 Preparation of a Composition Containing Salt of Example 5 Polyaspartic Acid Gear Lapping Using a Composition Containing a This example describes the preparation of a composition 30 Salt of Polyaspartic Acid and Grains/Grits containing at least 9% by weight of a salt of polyaspartic acid. This composition was prepared by combining water (7000g), The gear lapping was performed on equipment manufac the sodium salt of polyaspartic acid (735 g in 40% concen tured by Gleason Works. The pattern of motion for the gear tration and 830 g in 80% concentration), sodium 3-nitroben lapping was three dimensional, namely in the direction of G, Zenesulfonate (45g), citric acid (500g), Sodium tripolyphos 35 H, and V, which is readily understood by those skilled in the phate (375 g), anhydrous monosodium phosphate (45 g), art. The operating pressure varied from about 1 to about 3000 disodium dihydrogen pyrophosphate (280g), and carboxym psi. The lapping composition prepared as described in ethylcellulose (190 g). The solution was stirred for 6 hours to Example 4 was Supplied from an individual tank attached to provide a clear Solution. the lapping machine and was introduced to the meshing tooth 40 Surface of two gears under load conditions through nozzles Example 2 near the meshing point of the teeth. The exact motion pattern Metal Surface Finishing Using a Composition and duration were based on the existing gear production Containing a Salt of Polyaspartic Acid protocol using oil based lapping compounds known in the art. 45 After the operation, the processed gears were simply rinsed The composition prepared as described in Example 1 was with water and mounted onto testing equipment to examine applied to a metal Substrate in a vibratory bow using ceramic both the lapping pattern and by noise level. If necessary, the media. After 2 hours of vibration, the surface smoothness of described lapping procedure was repeated, and progress of the processed metal substrate was better than metal substrates lapping was examined again with the testing equipment. that were processed using the composition of Example 1, but 50 The data illustrated that the composition was effective as a lacking the Sodium salt of polyaspartic acid. lapping and polishing composition. Specifically, this compo sition was effective at lapping gears to produce a set of gears Example 3 with a desirable lapping pattern. In addition, the lapped gears using the compositions reduced noise levels and were only Gear Lapping Using a Composition Containing a 55 one-fifth as noisy as the gears lapped using oil-based lapping Salt of Polyaspartic Acid compositions available in the art. The gear lapping was performed on equipment manufac Example 6 tured by Gleason Works. The pattern of motion for the gear lapping was three dimensional, namely in the direction of G, 60 H, and V, which is readily understood by those skilled in the Reusing a Spent Composition for Lapping Gears art. The operating pressure varied from about 1 to about 3000 psi. The lapping composition prepared as described in The spent composition from Example 5 is collected and the Example 1 was Supplied from an individual tank attached to components are analyzed by techniques known to those in the the lapping machine and was introduced to the meshing tooth 65 art. The composition is then modified by adding additional Surface of two gears under load conditions through nozzles components to ensure that the required components of the near the meshing point of the teeth. The exact motion pattern composition as set forth in Example 4 are present and the US 7,820,068 B2 17 18 mixture stirred. The mixture is then utilized in another pro (e) about 0.1% by weight of anhydrous monosodium pyro cess of lapping gears, as described in Example 5. phosphate; (f) about 1% by weight of disodium dihydrogen pyrophos Example 7 phate: (g) about 68% by weight of Zirconium, aluminum, and Recycling Components of a Spent Lapping hafnium oxides; Composition (h) about 0.6% by weight of sodium carboxymethylcellu lose; and The spent composition (100g) from Example 5 was diluted (i) about 0.1% by weight of sodium 3-nitrobenzene with water (400 g) and then subjected to centrifugation. The 10 Sulfonate. aqueous Solution was decanted and the loose grains and grits 9. The composition according to claim 7, consisting of were operationally washed and dried. These recovered loose (a) about 10 to about 30% by weight of water; grains and grits were ready for reuse in the preparation of a (b) about 0.01 to about 12% by weight of the sodium salt of new lapping composition. polyaspartic acid; 15 (c) about 0.01 to about 10% by weight of citric acid; Example 8 (d) about 0.01 to about 5% by weight of sodium tripoly phosphate; Recycling Components of a Spent Lapping (e) about 0.01 to about 5% by weight of anhydrous mono Composition Sodium pyrophosphate; (f) about 0.01 to about 5% by weight of disodium dihydro The spent composition (100g) from Example 5 was diluted gen pyrophosphate: with water (400 g) and then subjected to filtration. The recov (g) about 0.01 to about 2% by weight of sodium carboxym ered loose grains and grits were operationally washed and ethylcellulose; dried. These recovered loose grains and grits were ready for (h) about 0.01% to about 3% by weight of sodium 3-ni reuse in the preparation of a new lapping composition. 25 trobenzenesulfonate; and All publications cited in this specification are incorporated (i) about 25% to about 75% by weight of zirconium, alu herein by reference. While the invention has been described minum, and hafnium oxides. with reference to particular embodiments, it will be appreci 10. A composition consisting of: ated that modifications can be made without departing from (i) about 10 to about 30% by weight of water; the spirit of the invention. Such modifications are intended to 30 (ii) about 0.01 to about 12% by weight of the sodium salt of fall within the scope of the appended claims. polyaspartic acid; What is claimed is: (iii) about 0.01 to about 10% by weight of oxalic acid: 1. A composition consisting of a salt of polyaspartic acid, (iv) about 0.01 to about 5% by weight of sodium tripoly Sodium 3-nitrobenzenesulfonate, citric acid, Sodium tripoly phosphate; phosphate, anhydrous monosodium phosphate, disodium 35 (v) about 0.01 to about 5% by weight of anhydrous mono dihydrogen pyrophosphate, and sodium carboxymethylcellu Sodium pyrophosphate; lose. (vi) about 0.01 to about 5% by weight of disodium dihy 2. The composition according to claim 1, wherein said salt drogen pyrophosphate: of polyaspartic acid is the Sodium salt of polyaspartic acid. (vii) about 0.01 to about 2% by weight of sodium car 3. The composition according to claim 1, consisting of at 40 boxymethylcellulose; least about 9% by weight of a salt of polyaspartic acid. (viii) about 0.01% to about 3% by weight of sodium 3-ni 4. The composition according to claim 1, consisting of at trobenzenesulfonate; and least about 9.5% by weight of a salt of polyaspartic acid. (ix) about 25% to about 75% by weight of a grit. 5. A product consisting of 11. A composition consisting of: (i) a container consisting of the composition of claim 1; and 45 (ii) a container consisting of one or more of a grit. (a) about 10 to about 30% by weight of water; 6. A composition consisting of a salt of polyaspartic acid, a (b) about 0.01 to about 12% by weight of the sodium salt of grit, sodium 3-nitrobenzenesulfonate, citric acid, Sodium tri polyaspartic acid; polyphosphate, anhydrous monosodium phosphate, diso (c) about 0.01 to about 10% by weight of citric acid; dium dihydrogen pyrophosphate, and sodium carboxymeth (d) about 0.01 to about 5% by weight of sodium tripoly ylcellulose. 50 phosphate; 7. A composition consisting of water, a salt of polyaspartic (e) about 0.01 to about 5% by weight of anhydrous mono acid, Sodium 3-nitrobenzenesulfonate, citric acid, Sodium tri Sodium pyrophosphate; polyphosphate, anhydrous monosodium phosphate, diso (f) about 0.01 to about 5% by weight of disodium dihydro dium dihydrogen pyrophosphate, a grit, and sodium car 55 gen pyrophosphate: boxymethyl cellulose. (g) about 0.01 to about 2% by weight of sodium carboxym 8. The composition according to claim 7, consisting of: ethylcellulose; (a) about 24.4% by weight of water; (h) about 0.01% to about 3% by weight of sodium 3-ni (b) about 3% by weight of the sodium salt of polyaspartic trobenzenesulfonate; and acid; 60 (i) about 25% to about 75% by weight of a grit. (c) about 1.6% by weight of citric acid; (d) about 1.2% by weight of sodium tripolyphosphate: k k k k k