WO2006018519A2 - Abrasive grit with high alumina content grain in particular for application in applied and sintered abrasives for example in scarfing grinders for slabs of steel alloys - Google Patents
Abrasive grit with high alumina content grain in particular for application in applied and sintered abrasives for example in scarfing grinders for slabs of steel alloys Download PDFInfo
- Publication number
- WO2006018519A2 WO2006018519A2 PCT/FR2005/001898 FR2005001898W WO2006018519A2 WO 2006018519 A2 WO2006018519 A2 WO 2006018519A2 FR 2005001898 W FR2005001898 W FR 2005001898W WO 2006018519 A2 WO2006018519 A2 WO 2006018519A2
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- WO
- WIPO (PCT)
- Prior art keywords
- weight
- abrasive
- typically
- titanium oxide
- alumina
- Prior art date
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
- C09K3/1418—Abrasive particles per se obtained by division of a mass agglomerated by sintering
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
- C04B35/111—Fine ceramics
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
- C04B2235/3267—MnO2
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5427—Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5463—Particle size distributions
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/78—Grain sizes and shapes, product microstructures, e.g. acicular grains, equiaxed grains, platelet-structures
- C04B2235/786—Micrometer sized grains, i.e. from 1 to 100 micron
Definitions
- the invention relates to the field of sintered abrasive grains used for the production of abrasive tools. It relates more particularly to the field of agglomerated abrasives and that of abrasives applied.
- the agglomerated abrasives are intended for the production of products in which the abrasive grains are dispersed in a resin-based binder, typically grinding wheels.
- the abrasives applied are typically abrasive powders deposited on supports (paper, canvas, tape, etc.).
- the present invention is more particularly intended for the manufacture of agglomerated abrasives, such as those used for the production of grinding wheels for the cutting of steel slabs, deburring casting or even metal grinding. These agglomerated abrasives will subsequently be used to illustrate the invention.
- the agglomerated abrasives and the abrasives applied are prepared from abrasive grains which can be, depending on the case, obtained either by grinding a product called "rock" consisting of a solid product resulting from the solidification of a liquid product , for example an electrofused abrasive such as corundum, or by sintering a powder consisting of grains whose composition and geometric shape favor good abrasive properties, or else by the "sol-gel" process described for example in the US Pat. US 4,574,003 (3M).
- the abrasive grains must have good mechanical properties, such as toughness or strength and good cutting power.
- the solidity characterizes the propensity of the grain to fracture by generating fragments under the effect of a mechanical stress.
- the tested product is calibrated according to the grade to be tested. After mechanical stressing (rotation in a jar loaded with steel balls), the sample is sieved along a column of several sieves whose meshes have been predefined. A specific coefficient is assigned to each recovered fraction, which makes it possible to classify the performance of the quality in terms of solidity, expressed as a barycentric average of the contents relative to each fraction [expressed in%]. The higher the strength, the higher the value obtained must be close to 100. An example is given at the end of the document for the determination of the strength of a grade 12 grain (that is to say having an initial size of between 1, 7 and 2 mm).
- the hardness characteristic of the plastic deformation of the material subjected to indentation is a criterion that is certainly necessary but insufficient to characterize the strength of an abrasive grain.
- a very hard grain can be fragile and its breakage can have a beneficial effect (the appearance of new sharp edges for example) but also negative effects (lower cutting power, poor finish, etc.).
- a less hard grain can be less fragile and ultimately prove more apt to "regenerate its edges".
- G (amount of material removed) / (amount of used abrasive).
- certain conditions of use such as the cutting of alloy steel slabs, may require from the abrasive grain that it gives the agglomerated product a cutting performance of the order of 200 to 2000kg / h undergoing a very high pressure (up to 55 daN / cm2 in extreme conditions) coupled to a peripheral temperature up to 1000 0 C.
- abrasive products available on the market includes: • corundums, white or brown, electro-fused, which have the disadvantage of being friable;
- grinding wheels are generally used. based on corundum-zirconia (typically comprising 25% ZrO2) but such grinding wheels are unsuitable for finishing, so that it is necessary to use successively several types of abrasives to carry out the process of scribing. - AT -
- the applicant has therefore sought to obtain abrasive grains which have better properties - strength and cutting power - than the market products, with the exception of grains obtained by the sol-gel process.
- the goal is to get closer to the properties of the latter, which certainly have good strength and good cutting power but the cost of obtaining is prohibitive for a large number of applications.
- An object of the invention is an abrasive grain containing essentially sintered alumina, characterized in that it comprises more than 96% by weight of alumina, between 0.1% and 3% by weight of titanium oxide and between 0.1% and 3%
- the whole titanium oxide + manganese oxide remaining less than 4% by weight.
- the weight content of titanium oxide and / or of manganese oxide is greater than or equal to 0.5%.
- the weight content of titanium oxide and / or manganese oxide is 0 less than or equal to 1.3%.
- the Applicant has in fact discovered that by adding a small proportion of titanium oxide and manganese oxide, the alumina could be, with equivalent abrasive properties, sintered at a much lower temperature.
- the method according to the invention has the advantage of allowing the use of existing furnaces, used for example until now for the sintering of bauxite.
- the invention provides a low sintering temperature which allows the use of a treatment furnace parade, reduced investment, easy control and 0 can handle high flow rates. This is for example a rotary kiln coated with refractories and operating continuously.
- the sintering time is Relatively low, of the order of 20 minutes at the bearing, which involves a complete cycle (temperature rise - bearing at the sintering temperature - cooling) of between 30 and 120 minutes, typically 90 minutes cold to cold.
- the addition of a significant amount of sintering additives introduces phases which, precipitated in the vicinity of the grain boundaries, are sources of weakness of the abrasive product. For this reason, the addition is, in practice, limited to levels of the order of 0.2% (see below the high temperature sintered alumina of Example 2, which contains 0.2% magnesia).
- the Applicant has found that, surprisingly, the addition of titanium oxide and manganese oxide (s) in a significant amount, greater than 0.1% for each of the oxides, allows to maintain the performance of the product regardless of its temperature of use.
- the manganese oxide and the titanium oxide must be present in the sintered alumina powder, at least 0.1% and at most 3% by weight for each of these types of oxides and at most 4% by weight for the whole.
- the manganese oxide may be present as MnO or MnO2. Its weight content is expressed in terms of MnO.
- the weight content of titanium oxide is greater than or equal to 0.5% and / or the weight content of manganese oxide (s) (expressed in terms of MnO) is greater than or equal to 0.5%.
- the weight content of titanium oxide is less than or equal to 1.3% and / or the weight content of manganese oxide (s) (expressed as MnO term) is less than or equal to 1, 3%.
- the weight content of titanium oxide and manganese oxide (s) is approximately equal to the weight content of titanium oxide, with a ratio typically between 0.8 and 1.2.
- the alumina particles are preferably alpha alumina and preferably come from calcined alumina, with a median diameter of about 2 ⁇ m.
- the grains obtained after sintering consist of particles of alumina compound / manganese oxide (s) / titanium oxide which have a homogeneous size, close to 10 microns, typically between 5 microns and 20 microns.
- Another object of the invention is an abrasive grain manufacturing process characterized by the following successive steps: a) producing a mixture comprising: a) a powder of calcined alumina grains whose crystallites have a mean diameter (expressed by the D50) between 1 ⁇ m, preferably 1.5 ⁇ m, and
- a2) a titanium oxide powder (TiO2), added to the mixture in a weight ratio of 0.1% to 3% and whose particle D50 is close to that of the alumina powder, for example between 1 and 3 ⁇ m, typically 2 ⁇ m; a3) a manganese oxide powder (MnO and / or MnO2) added to the mixture in a weight ratio of 0.1% to 3% and whose particle D50 is close to that of the alumina powder, for example between 1 and 3 ⁇ m, typically 2 ⁇ m; the mixture being homogenized mechanically, typically by kneading; b) Pressurized agglomeration of the powder thus obtained, in order to obtain bodies of green dough; c) Drying of raw dough bodies; d) Cooking at a temperature below 1600 ° C.
- TiO2 titanium oxide powder
- the firing temperature is close to 1500 0 C, typically between 1450 0 C and 155O 0 C.
- the complete cycle (temperature rise - bearing at the sintering temperature - cooling) is between 30 and 120 minutes, typically 90 minutes from cold to cold.
- the oven used is a rotary kiln operating continuously.
- the abrasive grain thus obtained is characterized by its density, strength and tearing performance. Its microstructure is controlled so as to obtain after cooking a particle size of the alumina compounds / manganese oxide (s) / homogeneous titanium oxide, close to 10 microns.
- the pressurized agglomeration of the powder is a compacting by dry spinning, resulting in the creation of fibers which are then broken so that it is possible to obtain bodies of raw dough in the form of prisms of given section. and of given height.
- Table I shows, for three calcined aluminas of different particle size, the strength values obtained after sintering at 1600 and 1650 ° C. It is noted that it is the alumina having the finest particle size which has the best values of solidity, However, the values are insufficient, the goal being to exceed 75.
- Table 2 shows the strength values measured for various products available on the market and, in the last column, for a product according to the invention.
- the strength values provided correspond to product quality averages, given that the individual values typically oscillate by + or - 5 with respect to these average values.
- the high temperature sintered alumina has a particle size similar to that of the product C set forth above and comprises a magnesia sintering agent. It was sintered at a temperature above 1600 ° C.
- the sintered alumina doped with the titanium and manganese oxides according to the present invention comprises 1.2% by weight of TiO 2 and 1.2% by weight of manganese oxide, expressed in terms of MnO. It has been sintered at 1500 ° C. It has a solidity that is clearly superior to the other sintered alumina. It has a lower solidity than sol-gel alumina but its cost is six times lower. It also has a lower strength than corundum-zirconia but is more suitable for finishing grinding.
- the basic sample is calibrated by selecting grains between 1.7 and 2 mm by sieving between two sieves (1, 7 and 2 mm of mesh size).
- the sieve column used comprises the following sieves defined by their mesh size: 1; 0.5; 0.25 and 0.125 mm
- the previous value is divided by the sum of the weighting coefficients. It can be seen from this formula that the larger the pass of the last sieve (0 gra in ⁇ 0.125 mm in this case), the lower the value obtained: the corresponding abrasive fragmented a lot, generated a large number of fines and therefore gets a lower value of strength.
Abstract
Description
Claims
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2007521989A JP2008507604A (en) | 2004-07-23 | 2005-07-22 | Abrasive grains with high alumina content especially for use in coated abrasives and agglomerated abrasives such as grinding grinders for alloy steel slabs |
EP05793370A EP1773732A2 (en) | 2004-07-23 | 2005-07-22 | Abrasive grit with high alumina content grain in particular for application in applied and sintered abrasives for example in scarfing grinders for slabs of steel alloys |
US11/631,670 US20070277444A1 (en) | 2004-07-23 | 2005-07-22 | Abrasive grit with high alumina content grain, in particular for application in applied and sintered abrasives, for example in scarfing grinders for slabs of steel alloy |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR0408197 | 2004-07-23 | ||
FR0408197A FR2873383B1 (en) | 2004-07-23 | 2004-07-23 | ABRASIVE GRAIN WITH HIGH ALUMINUM CONTENT, IN PARTICULAR FOR APPLICATIONS OF APPLIED AND AGGLOMERATED ABRASIVES, FOR EXAMPLE OF DECRYPING GRINDERS OF ALLIED STEEL BRUSHES |
Publications (2)
Publication Number | Publication Date |
---|---|
WO2006018519A2 true WO2006018519A2 (en) | 2006-02-23 |
WO2006018519A3 WO2006018519A3 (en) | 2006-08-03 |
Family
ID=34952452
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/FR2005/001898 WO2006018519A2 (en) | 2004-07-23 | 2005-07-22 | Abrasive grit with high alumina content grain in particular for application in applied and sintered abrasives for example in scarfing grinders for slabs of steel alloys |
Country Status (6)
Country | Link |
---|---|
US (1) | US20070277444A1 (en) |
EP (1) | EP1773732A2 (en) |
JP (1) | JP2008507604A (en) |
CN (1) | CN1989083A (en) |
FR (1) | FR2873383B1 (en) |
WO (1) | WO2006018519A2 (en) |
Families Citing this family (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
BRPI1009360A2 (en) * | 2009-03-11 | 2016-03-08 | Saint Gobain Abrasifs Sa | abrasive articles including fused zirconia alumina grains having an improved shape |
FR2948934B1 (en) * | 2009-08-05 | 2011-07-29 | Saint Gobain Ct Recherches | FROZEN ALUMINA-ZIRCONE GRAINS. |
DE102013111006B4 (en) * | 2013-10-04 | 2015-10-22 | Center For Abrasives And Refractories Research & Development C.A.R.R.D. Gmbh | Porous alumina-based polycrystalline Al 2 O 3 bodies with increased toughness |
DE102015103934A1 (en) * | 2014-04-17 | 2015-10-22 | Center For Abrasives And Refractories Research & Development C.A.R.R.D. Gmbh | An abrasive grain based on electrically molten alumina having a surface coating comprising titanium oxide and / or carbon |
CN105819833B (en) * | 2015-01-04 | 2019-02-05 | 江门市凯斯特尔实业有限公司 | A kind of preparation method from sharp type Fine Grain Alumina Ceramics abrasive grain |
CN109415616B (en) * | 2016-06-28 | 2021-03-19 | 昭和电工株式会社 | Fused alumina particles, method for producing fused alumina particles, grindstone, and abrasive cloth |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3454385A (en) * | 1965-08-04 | 1969-07-08 | Norton Co | Sintered alpha-alumina and zirconia abrasive product and process |
WO1994014722A1 (en) * | 1992-12-23 | 1994-07-07 | Minnesota Mining And Manufacturing Company | Abrasive grain containing manganese oxide |
US5651801A (en) * | 1993-11-12 | 1997-07-29 | Minnesota Mining And Manufacturing Company | Method for making an abrasive article |
US5690707A (en) * | 1992-12-23 | 1997-11-25 | Minnesota Mining & Manufacturing Company | Abrasive grain comprising manganese oxide |
-
2004
- 2004-07-23 FR FR0408197A patent/FR2873383B1/en not_active Expired - Fee Related
-
2005
- 2005-07-22 US US11/631,670 patent/US20070277444A1/en not_active Abandoned
- 2005-07-22 WO PCT/FR2005/001898 patent/WO2006018519A2/en active Application Filing
- 2005-07-22 CN CNA2005800244274A patent/CN1989083A/en active Pending
- 2005-07-22 JP JP2007521989A patent/JP2008507604A/en active Pending
- 2005-07-22 EP EP05793370A patent/EP1773732A2/en not_active Withdrawn
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3454385A (en) * | 1965-08-04 | 1969-07-08 | Norton Co | Sintered alpha-alumina and zirconia abrasive product and process |
WO1994014722A1 (en) * | 1992-12-23 | 1994-07-07 | Minnesota Mining And Manufacturing Company | Abrasive grain containing manganese oxide |
US5690707A (en) * | 1992-12-23 | 1997-11-25 | Minnesota Mining & Manufacturing Company | Abrasive grain comprising manganese oxide |
US5651801A (en) * | 1993-11-12 | 1997-07-29 | Minnesota Mining And Manufacturing Company | Method for making an abrasive article |
Also Published As
Publication number | Publication date |
---|---|
FR2873383A1 (en) | 2006-01-27 |
JP2008507604A (en) | 2008-03-13 |
FR2873383B1 (en) | 2006-10-06 |
CN1989083A (en) | 2007-06-27 |
WO2006018519A3 (en) | 2006-08-03 |
US20070277444A1 (en) | 2007-12-06 |
EP1773732A2 (en) | 2007-04-18 |
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