CA1074574A - Fused aluminum oxide abrasive grain containing reduced titanium oxide - Google Patents
Fused aluminum oxide abrasive grain containing reduced titanium oxideInfo
- Publication number
- CA1074574A CA1074574A CA277,176A CA277176A CA1074574A CA 1074574 A CA1074574 A CA 1074574A CA 277176 A CA277176 A CA 277176A CA 1074574 A CA1074574 A CA 1074574A
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- Canada
- Prior art keywords
- weight
- abrasive grain
- grain
- process according
- abrasive
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Classifications
-
- 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
- C09K3/1427—Abrasive particles per se obtained by division of a mass agglomerated by melting, at least partially, e.g. with a binder
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
- B24D3/02—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
- B24D3/20—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially organic
- B24D3/28—Resins or natural or synthetic macromolecular compounds
- B24D3/285—Reaction products obtained from aldehydes or ketones
Abstract
FUSED ALUMINUM OXIDE ABRASIVE GRAIN
CONTAINING REDUCED TITANIUM OXIDE
Abstract of the Disclosure A fused abrasive grain, useful for inclusion in coated abrasives and bonded abrasives, consists essentially of alumina; titanium oxide containing from about 0.42 to about 0.84% titanium, by weight of the abrasive grain, present as a reduced titanium oxide having an average oxidation state lower than in Ti2O3; from about 0.5 to about 0.3% by weight carbon; from about 0.02 to about 0.1% by weight Na2O; and from 0 to about 0.1% by weight total of calcium and silicon oxides. The grain before roasting has a gain on ignition of from about 0.4 to about 0.7% by weight, and is produced in an electric furnace by fusing high-purity titania, alumina con-taining Na2O as the only significant oxide impurity, and carbon, followed by crushing and roasting the fused grain.
CONTAINING REDUCED TITANIUM OXIDE
Abstract of the Disclosure A fused abrasive grain, useful for inclusion in coated abrasives and bonded abrasives, consists essentially of alumina; titanium oxide containing from about 0.42 to about 0.84% titanium, by weight of the abrasive grain, present as a reduced titanium oxide having an average oxidation state lower than in Ti2O3; from about 0.5 to about 0.3% by weight carbon; from about 0.02 to about 0.1% by weight Na2O; and from 0 to about 0.1% by weight total of calcium and silicon oxides. The grain before roasting has a gain on ignition of from about 0.4 to about 0.7% by weight, and is produced in an electric furnace by fusing high-purity titania, alumina con-taining Na2O as the only significant oxide impurity, and carbon, followed by crushing and roasting the fused grain.
Description
C15-2 Canada 745'~
FUSED ALUMINUM OXIDE ABRASIVE GRAIN
CONTAINING REDUCED TITANIUM OXIDE
Background of the Invention The abrasive industry constantly seeks new and improved abrasive grains for use in coated and bonded abrasive products.
It is therefore an obiect of this invention to provide an abrasive grain for such uses having improved performance characteristics. It is a further object of this invention to avoid the use of zirconia, for while prolific patent and other literature exists attesting to the utility of fused alumina-zirconia grain as an all-around abrasive for use in both coated and bonded products, zirconium oxide is subject to price variation and other problems.
Summary of the Invention Accordingly, the present invention provides a fused abrasive grain consisting essentially of titanium oxide con-taining from about 0.42 to about 0.84% titanium, by weight of the abrasive grain, the titanium being present as a reduced titanium oxide having an average oxidation state lower than in Ti203; from about 0.05 to about 0.3% by weight carbon; from about 0.02 to about 0.1% by weight Na20; from about O to about 0.1% by weight total calcium and silicon oxide; and alumina;
the abrasive having a gain on ignition in air at 1300C, when of a size of about 147 microns and finer, of from about 0.4 to about 0.7% by weight before roasting. Such a grain, useful for example in coated abrasives, with or without a base layer of abrasive grain of diverse composition, and in bonded abra-sives bonded with vitrified ceramic bonds or phenolic resin bonds, can be produced from high-purity titania, alumina con-taining soda as the only oxide impurity present in an amount in excess of 0.1% by weight, and carbon.
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Detailed Description This invention relates to a fused aluminum oxide abra-sive grain containing reduced titanium oxide. By "reduced"
titanium oxide, it is meant that the titanium oxide is present with an average oxidation state lower than that in Ti203, in contrast to the usual oxidation state of titanium in titanium dioxide, TiO2. This titanium oxide should be present in an amount such that there is from about 0.42 to about 0.84%
titanium, by weight of the abrasive grain. As titanium is usually analytically determined as TiO2, this means that the apparent TiO2 concentration should be from about 0.7 to about 1.4% by weight. This relationship obtains because TiO2 is abou~ 60.0% by weight titanium.
The second intentional additive ingredient of the abra-sive grain of the present invention is carbon. Carbon should be present in an amount from about 0.05 to about 0.3% by weight of the abrasive grain. Carbon is purposely added as part of the furnace charge in fusing the abrasive grain of the present invention, and according to the preferred process for producing the fused abrasive grain of the present invention, also enters the reaction mix from the carbon electrodes which are used in the electric furnace. The amount of carbon added depends upon the amount of titania and Na20 present in the reaction mix, as sufficient carbon is added at least tc reduce the titanium below its oxidation state in Ti203, and to reduce the Na20 to metallic sodium. The metallic sodium then vola-tilizes from the reaction mixture, being reconverted to Na20 when it leaves the reduc;ng atmosphere adjacent to the reac-tion zone of the furnace. Carbon monoxide, C0, is also given off as a by-product.
11~7457~
Sodium oxide is present as an impurity in the alumina, and should be controlled to less than about 0.1% by weight Na20. It is uneconomical to remove the last traces of Na20, and accordingly, a minimum concentration of 0.02% by weight Na20 is all that is economically feasible. The range of Na20 present in the fused abrasive grain according to the present invention should therefore range from about 0.02 to about 0.1%
by weight.
Calcium and silicon oxides are frequently present in alumina in minor degree. Their presence is not harmful if present at a level less than about 0.1% by weight.
The balance of the material is, of course, alumina.
An important feature of the present invention is the amount of gain on ignition. The gain on ignition is a measure of the oxidation state of the titanium oxide and of the amount of carbon present. While various conditions could be used for determining the gain on ignition, a standard which has been used in determining the proper oxidation state of the grain for the present invention is the gain on ignition in air at 1300C when the abrasive has been crushed and graded to a size of about 147 microns (100 mesh) and finer, and heated for 2 hours. This test is done before roasting the grain. The desired gain on ignition is from about 0.4 to about 0.7% by weight under these conditions.
Within the above broad limits, it is preferred that the fused abrasive grain according to the present invention con-sists essentially of titanium oxide containing about 0.72%
titanium, by weight of the abrasive grain, the titanium being present in an oxidation state lower than in Ti203 (which would be equivalent to 1.2% TiO2, if oxidized to TiO2); about 0.2% by weight carbon; about 0.05% by weight 1~37457~
Na20; and about 98.5% by weight A1203j the abrasive having a gain on ignition under the conditions specified above of about 0.5~ by weight.
The abrasive grain according to the present invention is useful in coated abrasive products such as belts and discs, as well as bonded abrasive products such as grinding wheels.
In the case of a coated abrasive product, the first component of the product is a flexible backing, such as paper or cloth.
The coated abrasive product also comprises abrasive grains comprising reduced titanium oxide according to the present invention, and an adhesive bonding the abrasive grain to the flexible backing. The adhesive is a conventional, and usually comprises a making coat of a conventional material such as phenolic resin containing a calcium carbonate filler, which serves to coat the flexible backing prior to application of the abrasive grain; and a size coat of conventional material such as phenolic resin containing a reactive filler, which serves to cover the making coat and the abrasive grain and more firmly bond the abrasive grain to the flexible backing. The abrasive grain used in such a coated abrasive product can either be entirely the abrasive grain comprising reduced titanium oxide according to the present invention, or can comprise in addition a base layer of abrasive grain, which is applied to the flexible backing having thereon a making adhe-sive coat, prior to application of the abrasive grain of thepresent invention. The use of a base coat of abrasive grain is conventional per se, and provides a substrate upon which the abrasive grains of the present invention can be mounted.
Bonded abrasives according to the present invention com-prise abrasive grain comprising reduced titanium oxide, as 1~74574 well as a bonding matrix of a conventional material such as phenolic resin or vitrified ceramic bond.
The preferred process for producing the fused abrasive grain according to the present invention comprises steps of charging an electric furnace; subjecting the mixture of ingredients within the electric furnace to the heat of an electric arc, to melt the mixture; solidifying the melted mixture; crushing the solidified mixture; and roasting the crushed grain. The mixture to be charged to the electric furnace preferably comprises from about 0.7 to about 1.7 parts by weight of high-purity titania, such as "electronic grade"
titania. It is preferred that the titania contain at least 99% TiO2, to avoid the introduction of unwanted impurities into the abrasive grain. A second raw material added to the furnace is preferably from about 98.6 to about 99.3 parts by weight of alumina containing Na20 as the only oxide impurity present in a significant amount (iOe., in excess of about 0.1%
by weight), for example tabular alumina having a maximum Na20 content of 0.15%. The Na20 content of the alumina raw material should be as low as convenient, as excess Na20 must be reduced be reaction with carbon to leave less than about 0.1% by weight Na20 in the finished product. Suitable alumina con-tains 0.3 - 0.6% Na20.
The third ingredient charged to the electric furnace of the present invention is carbon, such as calcined petroleum coke or graphite, in an amount from 1 to 10 times the theoret-ical amount necessary, based on the amount of TiO2 and Na20 added, to reduce the TiO2 and Na20. As used herein, the amount necessary to reduce the TiO2 and Na20 is considered according to the following formulas:
, :
.
, . . ~.
~074574 (i) 2TiO2 + C = Ti203 + C0, and (ii) Na20 + C = 2Na + C0.
It is to be recognized, of course, that the TiO2 will be reduced to an average titanium oxidation state less than in Ti203, and in particular it has been found that the average formula is more on the order of TiOo g- The reduction to the state Ti203 serves as a convenient benchmark in calculating the amount of carbon to add, however. The amount of carbon necessary to be added can be grossly estimated from the amount of TiO2 and Na20 present. By using carbon electrodes, however, additional carbon will be added to the reaction mixture from the carbon electrodes. It is also desirable to use additional carbon past the theoretical amount necessary to reduce the TiO2 and Na20 to Ti203 and Na, respectively, in an amount of from about 3 to 10 times the calculated amount. Within this range, from about 4 to 7 times the theoretical amount neces-sary, based on the amount of TiO2 and Na20 added, to reduce the TiO2 and Na20 to Ti203 and Na, respectively, ls preferred.
The carbon can be in any convenient form~ but finely divided calcined petroleum coke and graphite are preferred.
Various alumina sources can be used, but they should pre-ferably be of relatively high purity and contain no oxide impurities other than Na20 (or, of course, titanium oxides) in significant amounts, i.e., in excess of 0.1% by weight. An acceptable alumina source is calcined alumina, whlch can con-tain, for example, from about 0.4 to about 0.6% Na20 as an impurity.
According to the best mode now contemplated, the mixture of ingredients to be charged to the electric furnace comprises 1.4 parts by weight TiO2 (allowing 0.2 parts to settle to the bottom of the furnace as combined titanium compounds, leaving the equivalent of 1.2 parts TiO2 in the abrasive) and :
.
57~
98.5 parts by weight alumina containing Na20 as the only oxide impurity present in an amount in excess of 0.1% by weight. The amount of carbon to be added depends on the amount of Na20 present, as discussed above.
The mixture of titania, alumina and carbon is subjected within the electric furnace to the heat of an electric arc, the electric arc being a reducing arc passed from carbon elec-trodes to the mixture of titania, alumina, and carbon, for a time sufficient to melt the mixture. The term "reducing arc"
is well known to those skilled in the electric furnace art, and is a relatively short arc produced by controlling the power input, phase voltage, electrode spacing, power factor, circuit configuration (single-phase or three-phase), and the like. As an example, the electric arc can be supplied by a single-phase power supply at a voltage of about 80 volts and a power input of from about 100 to about 120 kilowatts.
After the mixture of titania, alumina and carbon is melted, it is solidified. It is highly preferred that this be accomplished by pouring the melted mixture into a cooling mold such as a water-cooled steel pan. A depth of melted mixture to be solidified of from about 2.5 to about 15 centi-meters, more particularly from about 2.5 to about 6 centi-meters, is preferred. An alternate cooling method is "ball casting", i.e., pouring the melted mixture into a solidifica-tion chamber containing steel spheres having a diameter ranging from about 5 to about 60 millimeters, more preferably of about 20 millimeters. Details of the ball casting process and apparatus for use therein are given in P. Cichy U. S.
Patent No. 3,726,621; W. Q. Richmond and P. Cichy U. S. Patents Nos. 3,861,849 and 3,928,515; W. Q. Richmond Canadian Patent ~7~5~
1,003,626; W. Q. Richmond and P. Cichy Canadian Patent 1,006,316; and P. Cichy Canadian Patent 1,006,315. All of the indicated patents are assigned to The Carborundum Company, the assignee of the present invention.
In any event, regardless of the cooling apparatus used, it is desired to prevent reoxidation of the reduced titanium oxide which is obtained by subjecting the mixture of titania, alumina and carbon to a reducing arc as indicated above. In order to prevent this reoxidation of the titanium, it is pre-ferred that the length of the pouring stream from the electric furnace to the cooling mold be minimized, and the pour rate maximized, insofar as practical.
After the melted mixture is solidified, it is crushed to obtain abrasive grain and "roasted" by subjecting the crushed grain to an oxidizing atmosphere, preferably air, for a time of from about 5 minutes to about 64 hours or more at a tem-perature of from about 1250C to about 1450C. The time of roasting more particularly is preferred to range from about 5 to about 20 minutes, optimum 10 minutes; and the temperature of roasting preferably ranges from about 1300 to about 1350C, optimum 1300C.
The product, as produced, should be bluish black in color. A reddish brown appearance indicates that the titanium is present in an oxidation state greater than desired. Such off-color material should be refurnaced to further reduce the titanium oxide present. The lumps exhibit a "glassy" con-choidal fracture which is suggestive of large crystal si~e.
1~174S74 The titanium may be combined with carbon and oxygen to form a titanium oxycarbide, and although the chemical identity of the titanium compounds present is not critical, the titanium must be present in a form which has a very low solubility in aluminum oxide. The titanium compound is present as an easily recognizable second phase, which may also contain aluminum oxide or aluminum oxycarbide. Freshly fractured crude abra-sive (i.e., solidified melt, prior to crushing to obtain abrasive grain) has a "carbidic" odor, a condition well known to those skilled in the art as indicative of over-reduction of the aluminum oxide fusion. This odor is produced upon contact with water of water vapor (or even high-humidity air).
The rate of cooling the melted mixture to solidify the same is rapid, in order to ensure that crystals grow in highly-oriented columns. Equivalent "grain" diameters of between .25 and about 2.5 millimeters, with a median of about 1.2 millimeters, have been observed. This is unusually large for thin cast alumina.
The "grains" (crystalline columns within an abrasive granule) exhibit a cellular substructure. The individual cells which have an equivalent diameter of between 0.06 and 0.1 millimeters are clearly outlined in photomicrographs of thin sections cut perpendicular to the direction of solidification, by the titanium-rich second phase. These cells appear to be alumina dendrites. These dentrites appear to be a stack of rhombohedral crystallite units which share a common "c" axis.
These columnar cells may, in some instances, be twinned stacks of rhombohedral units.
The structure of the abrasive grain of the present inven-tion is the result of the rate of solidification and the 57~
presence of an impurity phase which has a very low solubility in alumina. This impurity phase may limit lateral growth and branching of the dendrite columns. It has been established that, if the contained titanium is in a higher state of oxida-tion which permits solubility in alumina, the typical, desired cellular dendritic structure cannot be achieved at the solidi-fication conditions normally used.
Photomicrographs of sections cut parallel to the direc-tion of solidification reveal the columnar nature of the cell substructure of the primary grains. The minor impurity phase can be seen to be concentrated at the cell boundaries. In fact, it is precisely this impurity concentration which makes it possible to recognize the existence of the cellular sub-structure. In metallurgical practice the substructure ele-ments are sometimes called "impurity cells". These impurity cells, at low magnification, on planes parallel to the alumina "c" axis, sometimes exhibit a "feathery" or chevron pattern similar to that described by Baumann and Woodell in U. S.
Patent No. 2,383,n35.
During crushing, it has been observed that there is a distinct tendency for the large pieces to break more or less parallel to the direction of solidification. It appears that the grain fractures along the grain and cell boundaries, and it is believed that this fracture tendency will persist in the smaller granules which are incorporated into bonded and coated abrasive products. This property tends to favor production during crushing of elongated grit size particles which have a low bulk density. The particles also tend to have the very sharp, jagged edges and stepped fracture surfaces.
It has also been observed, qualitatively, that elongated ,. ~; ~ -, ~74~7~
fragments of the abrasive of the present invention have a high resistance to breaking in a direction perpendicular to the direction of solidification. This apparent anisotropy may also persist in final grit size particles. It is possible that it is a property of the "fiber bundle"-like structure described above.
The combination of high alpha alumina content, relatively low porosity and friability, plus a tendency to directional fracture with the production of exceptionally sharp, jagged, edges and faces, all result in high performance in certain abrasive applications. On coated abrasive products, both abrasive discs and abrasive belts, the grain of the present invention has performed from 15 to 90% better than standard bauxite-based alumina. In bonded abrasive products, particu-larly relatively thin "cut-off" wheels, 2 to 3 times standard grain performance has been demonstrated. .
The invention will now be illustrated with several examples.
A. Preparation of Grain Example 1 A tilting electric arc furnace was used, being equipped with two graphite electrodes for single-phase operation. The furnace has a nominal capacity of 100 kilowatts.
The charge to the furnace consists of high purity alumina, high purity titanium dioxide, and carbon in the form of graphite. The amount of carbon was calculated from the stoichiometric ratios for the reaction TiO2 -~ C = Ti203 + CO.
The weight ratio from this reaction is calculated at 7.51%, i.e., 7.51 grams of carbon for each 100 grams of TiO2. Using this ratio, 100% of the calculated stoichiometric amount of lV~74S74 carbon was used, based only on the TiO2 content. Since the tabular alumina contained a maximum of 0.05~ Na20, the Na20 required no reduction. The furnace charge was therefore cal-culated as 1.33 parts by weight of electronic grade titania;
S 0.10 parts by weight of graphite; and 98.57 parts by weight of tabular alumina containing a maximum of 0.05% Na20 (sold under the Alcoa designation "T61").
This mixture of titania, alumina and carbon was then sub-jected to the heat of an electric arc, the electric arc being a reducing arc passed from carbon electrodes to the mixture of titania, alumina and carbon, the voltage applied being 80 volts for a power input rate of 100-120 kilowatts. This voltage- power relationship was used to ensure a short "reducing" arc.
The charge ingredients were premixed and fed into the furnace at a rate of about 68 kilograms per hour to maintain a feed layer of unmelted ingredients approximately 2.5 centi-meters thick on top of the molten bath. This charge is almost completely melted down before pouring.
During pouring, the length of the pouring stream is mini-mized and the pour rate is maximized to limit the oxidation of the titanium oxide in the bath. The melted mixture was cast into a 52 centimeter diameter mold with steel walls and a 5 centimeter thick graphite base. Castings of from 2.5 to 10 centimeters were poured. Casting weights varied from about 13.6 to about 43.1 kilograms.
After the melted material has solidified, grain was pre-pared in a conventional manner by crushing cast material through a jaw crusher and roll crusher, followed by sieving to separate desired grit sizes. The grain was roasted in air 10 7457~
at a temperature of 1300C for 5 to 20 minute periods. Roast-ing decreased the ball mill friability (A.G.A. standard test procedure) and the bulk density of the 14 grit grain as set out in Table 1.
Table 1 Roasted Roasted Unroasted 5 20 Grain Minutes Minutes Bulk Density, g/cc 2.05 1.97 1.88 Friability % 29.2 22.4 20.1 Examples 2 - 5 Example 1 was repeated, using a standard roasting condi-tion and substituting calcined petroleum coke of 10-30 mesh size for the graphite of Example 1, and varying the propor-tions of ingredients to increase the ratio of carbon added tothe calculated stoichiometric amount as indicated in Example 1. For Examples 2-5, the roasting was for 10 minutes at 1300C.
The parts by weight of furnace charge for Examples 2-5, and the percentage of the calculated stoichiometric amount of carbon used, are set out in Table 2.
Table 2 Example 2 3 4 5 Alumina 98.5398.42 98.31 97.91 Titania 1.36 1.36 1.36 1.35 Carbon 0.11 0.22 0.33 0.74 Total Parts By Weight100.00100.00 100.00 100.00 Percent of Stoichio-metric Carbon 104 208 312 730 Examples 6 - 8 Example 1 was again repeated, substituting a tabular 1V~457~
alumina containing additional Na20 for the tabular alumina containing a maximum 0.05% Na20 of Example 1. Using the equation Na20 + C = 2Na + C0, the stoichiometric ratjo of carbon to Na20 was calculated at 19.4%, i.e., 19.4 grams carbon per 100 grams of Na20. The furnace charges were varied as set out in Table 3, taking account of the varying Na20 concentration.
Table 3 Example 6 7 8 10 Alumina 98.44 98.41 98.30 Titania 1.36 1.36 1.36 Carbon 0.20 0.23 0.34 Total Parts By Weight 100.00 100-00 100-00 15Percent of Stoichiometric Carbon 160 173 258 Example 9 Example 6 was again repeated, using 148% of the calcu-lated stoichiometric amount of carbon.
Example 10 - 15 The same procedure as set forth in Example 1 was followed except that the operating voltage was 100 volts and the average energy input was 150 kilowatts. The energy consump-tion was about 2.2 kw-hours per kilogram of melt poured.
Three melt cooling methods were applied, namely, cooling in sheets about 6.3 millimeters thick (Examples 10 and 11);
cooling in bricks about 10 centimeters thick (Examples 12 and 13); and cooling by casting into a bed of steel balls about 19 millimeters in diameter (Examples 14 and 15). The product after melting had the following analysis:
~-~74S7~
Titanium, determined as TiO2, 1.26%;*
Silica, SiO2, 0.03%
Soda, Na20, 0.02%;
Remainder assumed to be A1203.
*Actually present in an oxidatiGn state less than Ti203.
The indicated titanium concentration is 0.756% Ti.
The cooled crude abrasive was crushed separately to obtain grain samples. The bulk densities and standard fri-abilities of the material, of 14 grit size, together with the times and temperatures at which these materials were roasted, are set out in Table 4.
Table 4 Standard Bulk Friabil-Cooling Roasting Roasting Density, ity, Example Method Temp.Time g/ccPercent (1) 1350C5 min. 2.00 20.0 11 (1) 1350C20 min. 1.99 18.8 12 (2) 1350C5 min. 2.00 22.4 13 (2) 1350C20 min. 2.00 20.1 14 (3) 1300C10 min. 1.98 21.8 (3) 1300C4 hrs. 1.99 18.5 (1) Cast in 6.3 mm thick sheets.
FUSED ALUMINUM OXIDE ABRASIVE GRAIN
CONTAINING REDUCED TITANIUM OXIDE
Background of the Invention The abrasive industry constantly seeks new and improved abrasive grains for use in coated and bonded abrasive products.
It is therefore an obiect of this invention to provide an abrasive grain for such uses having improved performance characteristics. It is a further object of this invention to avoid the use of zirconia, for while prolific patent and other literature exists attesting to the utility of fused alumina-zirconia grain as an all-around abrasive for use in both coated and bonded products, zirconium oxide is subject to price variation and other problems.
Summary of the Invention Accordingly, the present invention provides a fused abrasive grain consisting essentially of titanium oxide con-taining from about 0.42 to about 0.84% titanium, by weight of the abrasive grain, the titanium being present as a reduced titanium oxide having an average oxidation state lower than in Ti203; from about 0.05 to about 0.3% by weight carbon; from about 0.02 to about 0.1% by weight Na20; from about O to about 0.1% by weight total calcium and silicon oxide; and alumina;
the abrasive having a gain on ignition in air at 1300C, when of a size of about 147 microns and finer, of from about 0.4 to about 0.7% by weight before roasting. Such a grain, useful for example in coated abrasives, with or without a base layer of abrasive grain of diverse composition, and in bonded abra-sives bonded with vitrified ceramic bonds or phenolic resin bonds, can be produced from high-purity titania, alumina con-taining soda as the only oxide impurity present in an amount in excess of 0.1% by weight, and carbon.
_l_ ~`~
~ 1~ 1 ~074S7~
Detailed Description This invention relates to a fused aluminum oxide abra-sive grain containing reduced titanium oxide. By "reduced"
titanium oxide, it is meant that the titanium oxide is present with an average oxidation state lower than that in Ti203, in contrast to the usual oxidation state of titanium in titanium dioxide, TiO2. This titanium oxide should be present in an amount such that there is from about 0.42 to about 0.84%
titanium, by weight of the abrasive grain. As titanium is usually analytically determined as TiO2, this means that the apparent TiO2 concentration should be from about 0.7 to about 1.4% by weight. This relationship obtains because TiO2 is abou~ 60.0% by weight titanium.
The second intentional additive ingredient of the abra-sive grain of the present invention is carbon. Carbon should be present in an amount from about 0.05 to about 0.3% by weight of the abrasive grain. Carbon is purposely added as part of the furnace charge in fusing the abrasive grain of the present invention, and according to the preferred process for producing the fused abrasive grain of the present invention, also enters the reaction mix from the carbon electrodes which are used in the electric furnace. The amount of carbon added depends upon the amount of titania and Na20 present in the reaction mix, as sufficient carbon is added at least tc reduce the titanium below its oxidation state in Ti203, and to reduce the Na20 to metallic sodium. The metallic sodium then vola-tilizes from the reaction mixture, being reconverted to Na20 when it leaves the reduc;ng atmosphere adjacent to the reac-tion zone of the furnace. Carbon monoxide, C0, is also given off as a by-product.
11~7457~
Sodium oxide is present as an impurity in the alumina, and should be controlled to less than about 0.1% by weight Na20. It is uneconomical to remove the last traces of Na20, and accordingly, a minimum concentration of 0.02% by weight Na20 is all that is economically feasible. The range of Na20 present in the fused abrasive grain according to the present invention should therefore range from about 0.02 to about 0.1%
by weight.
Calcium and silicon oxides are frequently present in alumina in minor degree. Their presence is not harmful if present at a level less than about 0.1% by weight.
The balance of the material is, of course, alumina.
An important feature of the present invention is the amount of gain on ignition. The gain on ignition is a measure of the oxidation state of the titanium oxide and of the amount of carbon present. While various conditions could be used for determining the gain on ignition, a standard which has been used in determining the proper oxidation state of the grain for the present invention is the gain on ignition in air at 1300C when the abrasive has been crushed and graded to a size of about 147 microns (100 mesh) and finer, and heated for 2 hours. This test is done before roasting the grain. The desired gain on ignition is from about 0.4 to about 0.7% by weight under these conditions.
Within the above broad limits, it is preferred that the fused abrasive grain according to the present invention con-sists essentially of titanium oxide containing about 0.72%
titanium, by weight of the abrasive grain, the titanium being present in an oxidation state lower than in Ti203 (which would be equivalent to 1.2% TiO2, if oxidized to TiO2); about 0.2% by weight carbon; about 0.05% by weight 1~37457~
Na20; and about 98.5% by weight A1203j the abrasive having a gain on ignition under the conditions specified above of about 0.5~ by weight.
The abrasive grain according to the present invention is useful in coated abrasive products such as belts and discs, as well as bonded abrasive products such as grinding wheels.
In the case of a coated abrasive product, the first component of the product is a flexible backing, such as paper or cloth.
The coated abrasive product also comprises abrasive grains comprising reduced titanium oxide according to the present invention, and an adhesive bonding the abrasive grain to the flexible backing. The adhesive is a conventional, and usually comprises a making coat of a conventional material such as phenolic resin containing a calcium carbonate filler, which serves to coat the flexible backing prior to application of the abrasive grain; and a size coat of conventional material such as phenolic resin containing a reactive filler, which serves to cover the making coat and the abrasive grain and more firmly bond the abrasive grain to the flexible backing. The abrasive grain used in such a coated abrasive product can either be entirely the abrasive grain comprising reduced titanium oxide according to the present invention, or can comprise in addition a base layer of abrasive grain, which is applied to the flexible backing having thereon a making adhe-sive coat, prior to application of the abrasive grain of thepresent invention. The use of a base coat of abrasive grain is conventional per se, and provides a substrate upon which the abrasive grains of the present invention can be mounted.
Bonded abrasives according to the present invention com-prise abrasive grain comprising reduced titanium oxide, as 1~74574 well as a bonding matrix of a conventional material such as phenolic resin or vitrified ceramic bond.
The preferred process for producing the fused abrasive grain according to the present invention comprises steps of charging an electric furnace; subjecting the mixture of ingredients within the electric furnace to the heat of an electric arc, to melt the mixture; solidifying the melted mixture; crushing the solidified mixture; and roasting the crushed grain. The mixture to be charged to the electric furnace preferably comprises from about 0.7 to about 1.7 parts by weight of high-purity titania, such as "electronic grade"
titania. It is preferred that the titania contain at least 99% TiO2, to avoid the introduction of unwanted impurities into the abrasive grain. A second raw material added to the furnace is preferably from about 98.6 to about 99.3 parts by weight of alumina containing Na20 as the only oxide impurity present in a significant amount (iOe., in excess of about 0.1%
by weight), for example tabular alumina having a maximum Na20 content of 0.15%. The Na20 content of the alumina raw material should be as low as convenient, as excess Na20 must be reduced be reaction with carbon to leave less than about 0.1% by weight Na20 in the finished product. Suitable alumina con-tains 0.3 - 0.6% Na20.
The third ingredient charged to the electric furnace of the present invention is carbon, such as calcined petroleum coke or graphite, in an amount from 1 to 10 times the theoret-ical amount necessary, based on the amount of TiO2 and Na20 added, to reduce the TiO2 and Na20. As used herein, the amount necessary to reduce the TiO2 and Na20 is considered according to the following formulas:
, :
.
, . . ~.
~074574 (i) 2TiO2 + C = Ti203 + C0, and (ii) Na20 + C = 2Na + C0.
It is to be recognized, of course, that the TiO2 will be reduced to an average titanium oxidation state less than in Ti203, and in particular it has been found that the average formula is more on the order of TiOo g- The reduction to the state Ti203 serves as a convenient benchmark in calculating the amount of carbon to add, however. The amount of carbon necessary to be added can be grossly estimated from the amount of TiO2 and Na20 present. By using carbon electrodes, however, additional carbon will be added to the reaction mixture from the carbon electrodes. It is also desirable to use additional carbon past the theoretical amount necessary to reduce the TiO2 and Na20 to Ti203 and Na, respectively, in an amount of from about 3 to 10 times the calculated amount. Within this range, from about 4 to 7 times the theoretical amount neces-sary, based on the amount of TiO2 and Na20 added, to reduce the TiO2 and Na20 to Ti203 and Na, respectively, ls preferred.
The carbon can be in any convenient form~ but finely divided calcined petroleum coke and graphite are preferred.
Various alumina sources can be used, but they should pre-ferably be of relatively high purity and contain no oxide impurities other than Na20 (or, of course, titanium oxides) in significant amounts, i.e., in excess of 0.1% by weight. An acceptable alumina source is calcined alumina, whlch can con-tain, for example, from about 0.4 to about 0.6% Na20 as an impurity.
According to the best mode now contemplated, the mixture of ingredients to be charged to the electric furnace comprises 1.4 parts by weight TiO2 (allowing 0.2 parts to settle to the bottom of the furnace as combined titanium compounds, leaving the equivalent of 1.2 parts TiO2 in the abrasive) and :
.
57~
98.5 parts by weight alumina containing Na20 as the only oxide impurity present in an amount in excess of 0.1% by weight. The amount of carbon to be added depends on the amount of Na20 present, as discussed above.
The mixture of titania, alumina and carbon is subjected within the electric furnace to the heat of an electric arc, the electric arc being a reducing arc passed from carbon elec-trodes to the mixture of titania, alumina, and carbon, for a time sufficient to melt the mixture. The term "reducing arc"
is well known to those skilled in the electric furnace art, and is a relatively short arc produced by controlling the power input, phase voltage, electrode spacing, power factor, circuit configuration (single-phase or three-phase), and the like. As an example, the electric arc can be supplied by a single-phase power supply at a voltage of about 80 volts and a power input of from about 100 to about 120 kilowatts.
After the mixture of titania, alumina and carbon is melted, it is solidified. It is highly preferred that this be accomplished by pouring the melted mixture into a cooling mold such as a water-cooled steel pan. A depth of melted mixture to be solidified of from about 2.5 to about 15 centi-meters, more particularly from about 2.5 to about 6 centi-meters, is preferred. An alternate cooling method is "ball casting", i.e., pouring the melted mixture into a solidifica-tion chamber containing steel spheres having a diameter ranging from about 5 to about 60 millimeters, more preferably of about 20 millimeters. Details of the ball casting process and apparatus for use therein are given in P. Cichy U. S.
Patent No. 3,726,621; W. Q. Richmond and P. Cichy U. S. Patents Nos. 3,861,849 and 3,928,515; W. Q. Richmond Canadian Patent ~7~5~
1,003,626; W. Q. Richmond and P. Cichy Canadian Patent 1,006,316; and P. Cichy Canadian Patent 1,006,315. All of the indicated patents are assigned to The Carborundum Company, the assignee of the present invention.
In any event, regardless of the cooling apparatus used, it is desired to prevent reoxidation of the reduced titanium oxide which is obtained by subjecting the mixture of titania, alumina and carbon to a reducing arc as indicated above. In order to prevent this reoxidation of the titanium, it is pre-ferred that the length of the pouring stream from the electric furnace to the cooling mold be minimized, and the pour rate maximized, insofar as practical.
After the melted mixture is solidified, it is crushed to obtain abrasive grain and "roasted" by subjecting the crushed grain to an oxidizing atmosphere, preferably air, for a time of from about 5 minutes to about 64 hours or more at a tem-perature of from about 1250C to about 1450C. The time of roasting more particularly is preferred to range from about 5 to about 20 minutes, optimum 10 minutes; and the temperature of roasting preferably ranges from about 1300 to about 1350C, optimum 1300C.
The product, as produced, should be bluish black in color. A reddish brown appearance indicates that the titanium is present in an oxidation state greater than desired. Such off-color material should be refurnaced to further reduce the titanium oxide present. The lumps exhibit a "glassy" con-choidal fracture which is suggestive of large crystal si~e.
1~174S74 The titanium may be combined with carbon and oxygen to form a titanium oxycarbide, and although the chemical identity of the titanium compounds present is not critical, the titanium must be present in a form which has a very low solubility in aluminum oxide. The titanium compound is present as an easily recognizable second phase, which may also contain aluminum oxide or aluminum oxycarbide. Freshly fractured crude abra-sive (i.e., solidified melt, prior to crushing to obtain abrasive grain) has a "carbidic" odor, a condition well known to those skilled in the art as indicative of over-reduction of the aluminum oxide fusion. This odor is produced upon contact with water of water vapor (or even high-humidity air).
The rate of cooling the melted mixture to solidify the same is rapid, in order to ensure that crystals grow in highly-oriented columns. Equivalent "grain" diameters of between .25 and about 2.5 millimeters, with a median of about 1.2 millimeters, have been observed. This is unusually large for thin cast alumina.
The "grains" (crystalline columns within an abrasive granule) exhibit a cellular substructure. The individual cells which have an equivalent diameter of between 0.06 and 0.1 millimeters are clearly outlined in photomicrographs of thin sections cut perpendicular to the direction of solidification, by the titanium-rich second phase. These cells appear to be alumina dendrites. These dentrites appear to be a stack of rhombohedral crystallite units which share a common "c" axis.
These columnar cells may, in some instances, be twinned stacks of rhombohedral units.
The structure of the abrasive grain of the present inven-tion is the result of the rate of solidification and the 57~
presence of an impurity phase which has a very low solubility in alumina. This impurity phase may limit lateral growth and branching of the dendrite columns. It has been established that, if the contained titanium is in a higher state of oxida-tion which permits solubility in alumina, the typical, desired cellular dendritic structure cannot be achieved at the solidi-fication conditions normally used.
Photomicrographs of sections cut parallel to the direc-tion of solidification reveal the columnar nature of the cell substructure of the primary grains. The minor impurity phase can be seen to be concentrated at the cell boundaries. In fact, it is precisely this impurity concentration which makes it possible to recognize the existence of the cellular sub-structure. In metallurgical practice the substructure ele-ments are sometimes called "impurity cells". These impurity cells, at low magnification, on planes parallel to the alumina "c" axis, sometimes exhibit a "feathery" or chevron pattern similar to that described by Baumann and Woodell in U. S.
Patent No. 2,383,n35.
During crushing, it has been observed that there is a distinct tendency for the large pieces to break more or less parallel to the direction of solidification. It appears that the grain fractures along the grain and cell boundaries, and it is believed that this fracture tendency will persist in the smaller granules which are incorporated into bonded and coated abrasive products. This property tends to favor production during crushing of elongated grit size particles which have a low bulk density. The particles also tend to have the very sharp, jagged edges and stepped fracture surfaces.
It has also been observed, qualitatively, that elongated ,. ~; ~ -, ~74~7~
fragments of the abrasive of the present invention have a high resistance to breaking in a direction perpendicular to the direction of solidification. This apparent anisotropy may also persist in final grit size particles. It is possible that it is a property of the "fiber bundle"-like structure described above.
The combination of high alpha alumina content, relatively low porosity and friability, plus a tendency to directional fracture with the production of exceptionally sharp, jagged, edges and faces, all result in high performance in certain abrasive applications. On coated abrasive products, both abrasive discs and abrasive belts, the grain of the present invention has performed from 15 to 90% better than standard bauxite-based alumina. In bonded abrasive products, particu-larly relatively thin "cut-off" wheels, 2 to 3 times standard grain performance has been demonstrated. .
The invention will now be illustrated with several examples.
A. Preparation of Grain Example 1 A tilting electric arc furnace was used, being equipped with two graphite electrodes for single-phase operation. The furnace has a nominal capacity of 100 kilowatts.
The charge to the furnace consists of high purity alumina, high purity titanium dioxide, and carbon in the form of graphite. The amount of carbon was calculated from the stoichiometric ratios for the reaction TiO2 -~ C = Ti203 + CO.
The weight ratio from this reaction is calculated at 7.51%, i.e., 7.51 grams of carbon for each 100 grams of TiO2. Using this ratio, 100% of the calculated stoichiometric amount of lV~74S74 carbon was used, based only on the TiO2 content. Since the tabular alumina contained a maximum of 0.05~ Na20, the Na20 required no reduction. The furnace charge was therefore cal-culated as 1.33 parts by weight of electronic grade titania;
S 0.10 parts by weight of graphite; and 98.57 parts by weight of tabular alumina containing a maximum of 0.05% Na20 (sold under the Alcoa designation "T61").
This mixture of titania, alumina and carbon was then sub-jected to the heat of an electric arc, the electric arc being a reducing arc passed from carbon electrodes to the mixture of titania, alumina and carbon, the voltage applied being 80 volts for a power input rate of 100-120 kilowatts. This voltage- power relationship was used to ensure a short "reducing" arc.
The charge ingredients were premixed and fed into the furnace at a rate of about 68 kilograms per hour to maintain a feed layer of unmelted ingredients approximately 2.5 centi-meters thick on top of the molten bath. This charge is almost completely melted down before pouring.
During pouring, the length of the pouring stream is mini-mized and the pour rate is maximized to limit the oxidation of the titanium oxide in the bath. The melted mixture was cast into a 52 centimeter diameter mold with steel walls and a 5 centimeter thick graphite base. Castings of from 2.5 to 10 centimeters were poured. Casting weights varied from about 13.6 to about 43.1 kilograms.
After the melted material has solidified, grain was pre-pared in a conventional manner by crushing cast material through a jaw crusher and roll crusher, followed by sieving to separate desired grit sizes. The grain was roasted in air 10 7457~
at a temperature of 1300C for 5 to 20 minute periods. Roast-ing decreased the ball mill friability (A.G.A. standard test procedure) and the bulk density of the 14 grit grain as set out in Table 1.
Table 1 Roasted Roasted Unroasted 5 20 Grain Minutes Minutes Bulk Density, g/cc 2.05 1.97 1.88 Friability % 29.2 22.4 20.1 Examples 2 - 5 Example 1 was repeated, using a standard roasting condi-tion and substituting calcined petroleum coke of 10-30 mesh size for the graphite of Example 1, and varying the propor-tions of ingredients to increase the ratio of carbon added tothe calculated stoichiometric amount as indicated in Example 1. For Examples 2-5, the roasting was for 10 minutes at 1300C.
The parts by weight of furnace charge for Examples 2-5, and the percentage of the calculated stoichiometric amount of carbon used, are set out in Table 2.
Table 2 Example 2 3 4 5 Alumina 98.5398.42 98.31 97.91 Titania 1.36 1.36 1.36 1.35 Carbon 0.11 0.22 0.33 0.74 Total Parts By Weight100.00100.00 100.00 100.00 Percent of Stoichio-metric Carbon 104 208 312 730 Examples 6 - 8 Example 1 was again repeated, substituting a tabular 1V~457~
alumina containing additional Na20 for the tabular alumina containing a maximum 0.05% Na20 of Example 1. Using the equation Na20 + C = 2Na + C0, the stoichiometric ratjo of carbon to Na20 was calculated at 19.4%, i.e., 19.4 grams carbon per 100 grams of Na20. The furnace charges were varied as set out in Table 3, taking account of the varying Na20 concentration.
Table 3 Example 6 7 8 10 Alumina 98.44 98.41 98.30 Titania 1.36 1.36 1.36 Carbon 0.20 0.23 0.34 Total Parts By Weight 100.00 100-00 100-00 15Percent of Stoichiometric Carbon 160 173 258 Example 9 Example 6 was again repeated, using 148% of the calcu-lated stoichiometric amount of carbon.
Example 10 - 15 The same procedure as set forth in Example 1 was followed except that the operating voltage was 100 volts and the average energy input was 150 kilowatts. The energy consump-tion was about 2.2 kw-hours per kilogram of melt poured.
Three melt cooling methods were applied, namely, cooling in sheets about 6.3 millimeters thick (Examples 10 and 11);
cooling in bricks about 10 centimeters thick (Examples 12 and 13); and cooling by casting into a bed of steel balls about 19 millimeters in diameter (Examples 14 and 15). The product after melting had the following analysis:
~-~74S7~
Titanium, determined as TiO2, 1.26%;*
Silica, SiO2, 0.03%
Soda, Na20, 0.02%;
Remainder assumed to be A1203.
*Actually present in an oxidatiGn state less than Ti203.
The indicated titanium concentration is 0.756% Ti.
The cooled crude abrasive was crushed separately to obtain grain samples. The bulk densities and standard fri-abilities of the material, of 14 grit size, together with the times and temperatures at which these materials were roasted, are set out in Table 4.
Table 4 Standard Bulk Friabil-Cooling Roasting Roasting Density, ity, Example Method Temp.Time g/ccPercent (1) 1350C5 min. 2.00 20.0 11 (1) 1350C20 min. 1.99 18.8 12 (2) 1350C5 min. 2.00 22.4 13 (2) 1350C20 min. 2.00 20.1 14 (3) 1300C10 min. 1.98 21.8 (3) 1300C4 hrs. 1.99 18.5 (1) Cast in 6.3 mm thick sheets.
(2) Cast in 10 cm thick bricks, 30.5 x 30.5 cm.
(3) Cast over 19 mm steel balls.
Examples 16 - 25 14 grit grain, produced as indicated above for Examples 10-15, was subjected to roasting at various temperatures and for various times. The bulk densities and standard friabili-ties of the grain are set forth in Table 5.
...
~07~S74 Table 5 Standard Bulk Friabil-Cooling Roasting Roasting Density, ity, 5 Example Method Temp. Time Hrs. g/cc Percent 16 (1) 1350C 16 2.03 13.2 17 (1) 1350C 64 2.03 13.4 18 (2) 1250C 1 1.99 19.2 19 (2) 1250C 3 1.99 18.4 (2) 1350C 1 1.99 18.1 21 (2) 1350C 3 1.99 18.1 22 (2) 1350C 6 - 14.5 23 (2) 1350C 16 - 15.2 24 (2) 1450C 1 1.99 18.1 (2) 1450C 3 1.98 18.6 (1) Cast in 6.3 mm thick sheets (2) Cast in 10 cm thick bricks, 30.5 x 30.5 cm.
B. Coated Abrasive Products Examples 26 - 27 Abrasive grain produced as indicated above for Examples 12, 13 and 18-25, but roasted for 10 minutes at 1300C, was incorporated into coated abrasive products as follows:
An appropriate amount of making adhesive, containing 50%
phenolic resin of approximately 70% solids content and 50%
of a finely divided calcium carbonate filler, having a vis-cosity of about 2300 cps, was coated onto a standard cloth backing material. The amount of making coat was varied depending upon the grit size of abrasive grain to be produced, as set out in Table 6.
After the cloth had been coated with the making coat, it was passed over a supply of abrasive grain according to the 1~74S7~
invention, as described above. Appropriate amounts of the proper size of grain, as set out in Table 6, were then coated onto the making coat by electrostatic coating, i.e., by charging the backing material and the abrasive grains with opposite electric charges, so that the abrasive grains are propelled into the coated abrasive backing material in the desired orientation, i.e., with the elongated direction of the grains being approximately perpendicular to the coated abra-sive backing.
The making coat was then dried and cured, to securely hold the grains on the cloth backing. A second adhesive or size coat, containing 50% phenolic resin of 70% solids content and 50% of a reactive filler, the size coat having a viscosity of about 1100 cps, was then applied. The amounts of size coat 15 are likewise set out in Table 6. The size coat was then dried and cured.
Table 6 Example 26 27 Grit Size 36 40 Making Coat 2 2 (Measured wet) 274 g/m 281 g/m Abrasive Grain888 g/m 784 g/m Size Coat 2 2 (Measured wet) 414 g/m 325 g/m The coated abrasive sheet material, made as above, was then fabricated into coated abrasive belts of a standard size, having 36 or 40 grit abrasives. These belts were subjected to grinding tests in order to determine the efficiency of the grain. A run of 36 grit material similar to Example 26 was made using conventional aluminum oxide grain. This material ~V7457~
was used for a control. In the case of 40 grit, a standard production run of material using similar materials and con-ventional aluminum oxide was used for a control. The belts were tested on a double spindle backstand polishing lathe with a constant pressure infeed device equipped with a 35.5 centi-meter diameter, 5 centimeter wide rubber contact wheel of 70A durometer hardness, having a land to groove ratio of 1:2.
For all tests described in Examples 26 and 27, the abrasive belt was turned at a rate to give 5000 surface feet per minute of contact. For all tests, the material ground was 1 inch by l inch cold rolled No. 1018 steel.
For the 36 grit test, the steel bar was fed into the coated abrasive belt with 36 pounds of force, resulting in 36 pounds per square inch of pressure. During each test, several steel bars were alternated in grinding. The steel bars were first weighed, then placed in the grinding machine for 30 seconds per contact, weighed again and water-cooled. This procedure was repeated with alternate steel bars and the test was continued until an individual contact cut 20 grams or less of steel. The number of cuts obtained with the coated abra-sive belt before reaching the level of 20 grams per cut, as well as the total amount of steel cut by the belt before reach-ing this level, are recorded as an indication of the grinding efficiency of that belt. The results of three belts of grain according to the invention and three belts of the standard aluminum oxide control are set out in Table 7.
3~()74S7~
Table 7 Grams of Number Average Grams Grain Type Steel Removed of Cuts of Steel/Cut Invention, Run 1 1485 21 70.7 Invention, Run 2 1484 21 70.7 Invention, Run 3 1467 20 73 3 Control, Run 1728 12 60.7 Control, Run 2734 13 61.2 Control, Run 3677 12 56.4 For Example 27, a similar test was performed with 40 grit abrasives, except that in the case of the finer 40 grit abra-sive material, the force applied was 53 pounds, giving a pressure of 53 pounds per square inch, and the contact time was only 20 seconds per contact instead of 30. The 40 grit tests were also terminated when 20 grams or less were cut in a 20-second contact. The results of three belts of grain according to the invention and three belts of a conventional aluminum oxide commercial standard are listed in Table 8.
Table 8 Grams of Number Average Grams Grain Type Steel Removed of Cuts of Steel/Cut Invention, Run 1 1269 30 42.3 Invention, Run 2 1318 30 43.9 Invention, Run 3 1215 29 41.9 Control, Run 1596 16 37.2 Control, Run 2627 18 34.8 Control, Run 3577 16 36.1 Examples 28 - 30 Additional abrasive material, produced as indicated above for Examples 8, 8 and 9, for Examples 28, 29 and 30, _l g ~V74S~7~
respectively, was incorporated into abrasive belts. In Example 28, the abrasive belts were double-coated by applying first a standard aluminum oxide grain, and then applying grain of the invention over the first coat of abrasive grain, thus using the aluminum oxide grain as a substrate. For Examples 29 and 30, a single coating of abrasive grain accord-ing to the invention was applied. For both 36 and 50 grit grain, a control of standard aluminum oxide grain, for which the coated abrasive was made in the same manner as indicated for Example 29 and 30, except for the grain type, was tested.
The results of the standard test of these abrasive belts are set forth in Table 9.
Table 9 Grams Removed In Standard Test Example 36 Grit50 Grit lO00 1061 Alumina Control 701 878 Examples 31 - 34 The same grains as used in Examples 28-30 were coated onto fiber to produce fiber coated abrasive discs. Example 31 was abrasive produced as indicated in Example 8, single coated.
Example 32 was abrasive produced as indicated in Example 8, double coated as indicated in Example 28. Example 33 was abrasive grain produced as indicated in Example 9, single coated. Example 34 was abrasive produced as indicated in Example 9, and double coated as indicated in Example 28. The control for these examples was a standard fiber disc similar to Examples 31 and 33, except that aluminum oxide abrasive 1(~74S~4 grain was substituted for the abrasive grain of the invention.
The results of a standard test for these fiber discs and the control are set out in Table 10.
Table 10 Grams Cut In Standard Test 50 Grit 50 Grit Example 36 Grit Lot "A'l Steel Lot "B" Steel Alumina Control 93 57 79 C. Bonded Abrasive Products Examples 35 - 44 Bonded abrasives were produced using abrasive grain of the invention using the same procedure as that used for con-ventional phenolic resin bonded grinding wheels. The grain was wetted in a mixer with a blend of furfural-cresol in an amount of 1 cubic centimeter of blend for each kilogram of mix; a liquid phenolic resin was then added to the mixer and dispersed on the wetted grain for 2 minutes; 75% of the powdered phenolic resin and all of the filler was added to the mixer and mixed for a few minutes. The remainder of the powdered phenolic resin was added over a period of a few minutes. The last step is the addition of up to 10 cubic centimeters per kilogram of powdered resin of creosote oil to control the characteristics of the mix. The formulation used was as set out in Table 11.
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Table 11 Weight Percent 14 Grit Abrasive 41.4 16 Grit Abrasive 20.7 20 Grit Abrasive 20.6 Liquid Phenolic Resin 3.0 Powdered Phenolic Resin 6.8 Filler 7.5 TOTAL: 100.0 The mix was then loaded into a mold and fiberglass rein-forcing was incorporated into the filling at appropriate intervals to give a strength capable of operating at 12,500 surface feet per minute. The assembled mold was pressed to a specific size, the wheel stripped, loaded on a curing bat, lugged, weighed and placed in an oven for curing. The curing was accomplished over a two-day period, with hold time of 9 hours at a maximum temperature of about 180C. The wheels were removed from the oven and finished to the appropriate tolerances.
By this manner, 20 x 2 x 12" wheels were made containing standard aluminum oxide abrasive and four types of abrasive according to the invention. These wheels were then run on a floor stand grinder operating at 12,500 surface feet per minute, grinding 1 inch x 2 inch faces of malleable iron with standard operator pressure. The results of this test are set forth in Table 12.
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In a similar manner, but with minor modifications in the mix formulation and the pressing and curing, 6 x 6 x 5/8-inch, type 11 wheels were made and finished. No glass reinforcing was used in the construction. The mix formulation was as set out in Table 13.
Table 13 Weight Percent 14 Grit Abrasive 41.5 16 Grit Abrasive 20.8 20 Grit Abrasive 20.7 Liquid Phenolic Resin3.5 Powdered Phenolic Resin8.S
Filler 5.0 TOTAL: 100.0 These wheels were evaluated by running on a portable air grinder operating at 6000 rpm, grinding a piece of flat cast steel for 30 minutes with a standard operator pressure. The results of this evaluation are set out in Table 14.
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Similarly, type 27 depressed center 7 x 1/4 x 7/8" wheels were mixed, molded, and cured, incorporating the standard glass fiber reinforcement. The formation used was 80% 24 grit abrasive, 3% liquid phenolic resin, 10% powdered phenolic resin, and 7% filler. These wheels were evaluated by running a portable air grinder operating at 6000 rpm, grinding 1-1/2 x 1-1/2" angle iron for 15 minutes with a standard operator pressure. The results of this test are set out in Table 15.
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$74 The same wheels were then evaluated grinding flat cast steel for 30 minutes, using the same grinder at normal operator pressure. The results are set out in Table 16.
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Examples 16 - 25 14 grit grain, produced as indicated above for Examples 10-15, was subjected to roasting at various temperatures and for various times. The bulk densities and standard friabili-ties of the grain are set forth in Table 5.
...
~07~S74 Table 5 Standard Bulk Friabil-Cooling Roasting Roasting Density, ity, 5 Example Method Temp. Time Hrs. g/cc Percent 16 (1) 1350C 16 2.03 13.2 17 (1) 1350C 64 2.03 13.4 18 (2) 1250C 1 1.99 19.2 19 (2) 1250C 3 1.99 18.4 (2) 1350C 1 1.99 18.1 21 (2) 1350C 3 1.99 18.1 22 (2) 1350C 6 - 14.5 23 (2) 1350C 16 - 15.2 24 (2) 1450C 1 1.99 18.1 (2) 1450C 3 1.98 18.6 (1) Cast in 6.3 mm thick sheets (2) Cast in 10 cm thick bricks, 30.5 x 30.5 cm.
B. Coated Abrasive Products Examples 26 - 27 Abrasive grain produced as indicated above for Examples 12, 13 and 18-25, but roasted for 10 minutes at 1300C, was incorporated into coated abrasive products as follows:
An appropriate amount of making adhesive, containing 50%
phenolic resin of approximately 70% solids content and 50%
of a finely divided calcium carbonate filler, having a vis-cosity of about 2300 cps, was coated onto a standard cloth backing material. The amount of making coat was varied depending upon the grit size of abrasive grain to be produced, as set out in Table 6.
After the cloth had been coated with the making coat, it was passed over a supply of abrasive grain according to the 1~74S7~
invention, as described above. Appropriate amounts of the proper size of grain, as set out in Table 6, were then coated onto the making coat by electrostatic coating, i.e., by charging the backing material and the abrasive grains with opposite electric charges, so that the abrasive grains are propelled into the coated abrasive backing material in the desired orientation, i.e., with the elongated direction of the grains being approximately perpendicular to the coated abra-sive backing.
The making coat was then dried and cured, to securely hold the grains on the cloth backing. A second adhesive or size coat, containing 50% phenolic resin of 70% solids content and 50% of a reactive filler, the size coat having a viscosity of about 1100 cps, was then applied. The amounts of size coat 15 are likewise set out in Table 6. The size coat was then dried and cured.
Table 6 Example 26 27 Grit Size 36 40 Making Coat 2 2 (Measured wet) 274 g/m 281 g/m Abrasive Grain888 g/m 784 g/m Size Coat 2 2 (Measured wet) 414 g/m 325 g/m The coated abrasive sheet material, made as above, was then fabricated into coated abrasive belts of a standard size, having 36 or 40 grit abrasives. These belts were subjected to grinding tests in order to determine the efficiency of the grain. A run of 36 grit material similar to Example 26 was made using conventional aluminum oxide grain. This material ~V7457~
was used for a control. In the case of 40 grit, a standard production run of material using similar materials and con-ventional aluminum oxide was used for a control. The belts were tested on a double spindle backstand polishing lathe with a constant pressure infeed device equipped with a 35.5 centi-meter diameter, 5 centimeter wide rubber contact wheel of 70A durometer hardness, having a land to groove ratio of 1:2.
For all tests described in Examples 26 and 27, the abrasive belt was turned at a rate to give 5000 surface feet per minute of contact. For all tests, the material ground was 1 inch by l inch cold rolled No. 1018 steel.
For the 36 grit test, the steel bar was fed into the coated abrasive belt with 36 pounds of force, resulting in 36 pounds per square inch of pressure. During each test, several steel bars were alternated in grinding. The steel bars were first weighed, then placed in the grinding machine for 30 seconds per contact, weighed again and water-cooled. This procedure was repeated with alternate steel bars and the test was continued until an individual contact cut 20 grams or less of steel. The number of cuts obtained with the coated abra-sive belt before reaching the level of 20 grams per cut, as well as the total amount of steel cut by the belt before reach-ing this level, are recorded as an indication of the grinding efficiency of that belt. The results of three belts of grain according to the invention and three belts of the standard aluminum oxide control are set out in Table 7.
3~()74S7~
Table 7 Grams of Number Average Grams Grain Type Steel Removed of Cuts of Steel/Cut Invention, Run 1 1485 21 70.7 Invention, Run 2 1484 21 70.7 Invention, Run 3 1467 20 73 3 Control, Run 1728 12 60.7 Control, Run 2734 13 61.2 Control, Run 3677 12 56.4 For Example 27, a similar test was performed with 40 grit abrasives, except that in the case of the finer 40 grit abra-sive material, the force applied was 53 pounds, giving a pressure of 53 pounds per square inch, and the contact time was only 20 seconds per contact instead of 30. The 40 grit tests were also terminated when 20 grams or less were cut in a 20-second contact. The results of three belts of grain according to the invention and three belts of a conventional aluminum oxide commercial standard are listed in Table 8.
Table 8 Grams of Number Average Grams Grain Type Steel Removed of Cuts of Steel/Cut Invention, Run 1 1269 30 42.3 Invention, Run 2 1318 30 43.9 Invention, Run 3 1215 29 41.9 Control, Run 1596 16 37.2 Control, Run 2627 18 34.8 Control, Run 3577 16 36.1 Examples 28 - 30 Additional abrasive material, produced as indicated above for Examples 8, 8 and 9, for Examples 28, 29 and 30, _l g ~V74S~7~
respectively, was incorporated into abrasive belts. In Example 28, the abrasive belts were double-coated by applying first a standard aluminum oxide grain, and then applying grain of the invention over the first coat of abrasive grain, thus using the aluminum oxide grain as a substrate. For Examples 29 and 30, a single coating of abrasive grain accord-ing to the invention was applied. For both 36 and 50 grit grain, a control of standard aluminum oxide grain, for which the coated abrasive was made in the same manner as indicated for Example 29 and 30, except for the grain type, was tested.
The results of the standard test of these abrasive belts are set forth in Table 9.
Table 9 Grams Removed In Standard Test Example 36 Grit50 Grit lO00 1061 Alumina Control 701 878 Examples 31 - 34 The same grains as used in Examples 28-30 were coated onto fiber to produce fiber coated abrasive discs. Example 31 was abrasive produced as indicated in Example 8, single coated.
Example 32 was abrasive produced as indicated in Example 8, double coated as indicated in Example 28. Example 33 was abrasive grain produced as indicated in Example 9, single coated. Example 34 was abrasive produced as indicated in Example 9, and double coated as indicated in Example 28. The control for these examples was a standard fiber disc similar to Examples 31 and 33, except that aluminum oxide abrasive 1(~74S~4 grain was substituted for the abrasive grain of the invention.
The results of a standard test for these fiber discs and the control are set out in Table 10.
Table 10 Grams Cut In Standard Test 50 Grit 50 Grit Example 36 Grit Lot "A'l Steel Lot "B" Steel Alumina Control 93 57 79 C. Bonded Abrasive Products Examples 35 - 44 Bonded abrasives were produced using abrasive grain of the invention using the same procedure as that used for con-ventional phenolic resin bonded grinding wheels. The grain was wetted in a mixer with a blend of furfural-cresol in an amount of 1 cubic centimeter of blend for each kilogram of mix; a liquid phenolic resin was then added to the mixer and dispersed on the wetted grain for 2 minutes; 75% of the powdered phenolic resin and all of the filler was added to the mixer and mixed for a few minutes. The remainder of the powdered phenolic resin was added over a period of a few minutes. The last step is the addition of up to 10 cubic centimeters per kilogram of powdered resin of creosote oil to control the characteristics of the mix. The formulation used was as set out in Table 11.
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Table 11 Weight Percent 14 Grit Abrasive 41.4 16 Grit Abrasive 20.7 20 Grit Abrasive 20.6 Liquid Phenolic Resin 3.0 Powdered Phenolic Resin 6.8 Filler 7.5 TOTAL: 100.0 The mix was then loaded into a mold and fiberglass rein-forcing was incorporated into the filling at appropriate intervals to give a strength capable of operating at 12,500 surface feet per minute. The assembled mold was pressed to a specific size, the wheel stripped, loaded on a curing bat, lugged, weighed and placed in an oven for curing. The curing was accomplished over a two-day period, with hold time of 9 hours at a maximum temperature of about 180C. The wheels were removed from the oven and finished to the appropriate tolerances.
By this manner, 20 x 2 x 12" wheels were made containing standard aluminum oxide abrasive and four types of abrasive according to the invention. These wheels were then run on a floor stand grinder operating at 12,500 surface feet per minute, grinding 1 inch x 2 inch faces of malleable iron with standard operator pressure. The results of this test are set forth in Table 12.
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In a similar manner, but with minor modifications in the mix formulation and the pressing and curing, 6 x 6 x 5/8-inch, type 11 wheels were made and finished. No glass reinforcing was used in the construction. The mix formulation was as set out in Table 13.
Table 13 Weight Percent 14 Grit Abrasive 41.5 16 Grit Abrasive 20.8 20 Grit Abrasive 20.7 Liquid Phenolic Resin3.5 Powdered Phenolic Resin8.S
Filler 5.0 TOTAL: 100.0 These wheels were evaluated by running on a portable air grinder operating at 6000 rpm, grinding a piece of flat cast steel for 30 minutes with a standard operator pressure. The results of this evaluation are set out in Table 14.
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Similarly, type 27 depressed center 7 x 1/4 x 7/8" wheels were mixed, molded, and cured, incorporating the standard glass fiber reinforcement. The formation used was 80% 24 grit abrasive, 3% liquid phenolic resin, 10% powdered phenolic resin, and 7% filler. These wheels were evaluated by running a portable air grinder operating at 6000 rpm, grinding 1-1/2 x 1-1/2" angle iron for 15 minutes with a standard operator pressure. The results of this test are set out in Table 15.
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$74 The same wheels were then evaluated grinding flat cast steel for 30 minutes, using the same grinder at normal operator pressure. The results are set out in Table 16.
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Claims (28)
1. A fused abrasive grain consisting essentially of:
(1) titanium oxide containing from about 0.42 to about 0.84% titanium, by weight of the abrasive grain, said titanium being present as a reduced titanium oxide having an average oxidation state lower than in Ti2O3;
(2) from about 0.05 to about 0.3% by weight carbon;
(3) from about 0.02 to about 0.1% by weight Na2O;
(4) from 0 to about 0.1% by weight total of calcium and silicon oxides; and (5) alumina;
said abrasive having a gain on ignition in air before roasting at 1300°C, when of a size of about 147 microns and finer, of from about 0.4 to about 0.7% by weight.
(1) titanium oxide containing from about 0.42 to about 0.84% titanium, by weight of the abrasive grain, said titanium being present as a reduced titanium oxide having an average oxidation state lower than in Ti2O3;
(2) from about 0.05 to about 0.3% by weight carbon;
(3) from about 0.02 to about 0.1% by weight Na2O;
(4) from 0 to about 0.1% by weight total of calcium and silicon oxides; and (5) alumina;
said abrasive having a gain on ignition in air before roasting at 1300°C, when of a size of about 147 microns and finer, of from about 0.4 to about 0.7% by weight.
2. A fused abrasive grain according to claim 1, consisting essentially of:
(1) titanium oxide containing about 0.72% titanium, by weight of the abrasive grain;
(2) about 0.2% by weight carbon;
(3) about 0.05% by weight Na2O; and (4) about 98.5% by weight alumina;
and having a gain on ignition of about 0.5% by weight.
(1) titanium oxide containing about 0.72% titanium, by weight of the abrasive grain;
(2) about 0.2% by weight carbon;
(3) about 0.05% by weight Na2O; and (4) about 98.5% by weight alumina;
and having a gain on ignition of about 0.5% by weight.
3. A coated abrasive product comprising:
(1) a flexible backing;
(2) abrasive grain comprising reduced titanium oxide according to claim 1; and (3) adhesive bonding said abrasive grain to said backing.
(1) a flexible backing;
(2) abrasive grain comprising reduced titanium oxide according to claim 1; and (3) adhesive bonding said abrasive grain to said backing.
4. A coated abrasive product according to claim 3, wherein the flexible backing is cloth; the adhesive comprises a making coat of phenolic resin comprising a calcium carbonate filler and a size coat of phenolic resin comprising a reactive filler.
5. A coated abrasive product according to claim 4, comprising in addition a base layer of abrasive grain, under the abrasive grain comprising reduced titanium oxide.
6. A bonded abrasive product comprising:
(1) abrasive grain comprising reduced titanium oxide according to claim 1; and (2) a bonding matrix, bonding together the abrasive grain.
(1) abrasive grain comprising reduced titanium oxide according to claim 1; and (2) a bonding matrix, bonding together the abrasive grain.
7. A bonded abrasive product according to claim 6, wherein the bonding matrix is phenolic resin.
8. A bonded abrasive product according to claim 6, wherein the bonding matrix is vitrified ceramic bond.
9. A bonded abrasive product according to claim 6, in the form of a grinding wheel.
10. A process for producing a fused abrasive grain according to claim 1, comprising the steps of:
(1) charging to an electric furnace a mixture of:
(a) from about 0.7 to about 1.7 parts by weight high purity TiO2;
(b) from about 98.6 to about 99.3 parts by weight alumina containing Na2O as the only oxide impurity present in an amount in excess of 0.1% by weight; and (c) carbon, in an amount of from 1 to 10 times the theoretical amount necessary, based on the amount of TiO2 and Na2O added, to reduce the TiO2 and Na2O according to the following formulas:
(i) 2TiO2 + C = Ti2O3 + Co, and (ii) Na2O + C = 2NA + CO; and (2) subjecting the mixture of titania, alumina and carbon to the heat of an electric arc, said electric arc being a reducing arc passed from carbon electrodes to the mixture of titania, alumina and carbon, for a time sufficient to melt the mixture;
(3) solidfying the melted mixture;
(4) crushing the solidified mixture to obtain abrasive grain; and (5) roasting the abrasive grain by subjecting the crushed grain to an oxidizing atmosphere for from about 5 minutes to about 64 hours at a temperature of from about 1250°C to about 1450°C.
(1) charging to an electric furnace a mixture of:
(a) from about 0.7 to about 1.7 parts by weight high purity TiO2;
(b) from about 98.6 to about 99.3 parts by weight alumina containing Na2O as the only oxide impurity present in an amount in excess of 0.1% by weight; and (c) carbon, in an amount of from 1 to 10 times the theoretical amount necessary, based on the amount of TiO2 and Na2O added, to reduce the TiO2 and Na2O according to the following formulas:
(i) 2TiO2 + C = Ti2O3 + Co, and (ii) Na2O + C = 2NA + CO; and (2) subjecting the mixture of titania, alumina and carbon to the heat of an electric arc, said electric arc being a reducing arc passed from carbon electrodes to the mixture of titania, alumina and carbon, for a time sufficient to melt the mixture;
(3) solidfying the melted mixture;
(4) crushing the solidified mixture to obtain abrasive grain; and (5) roasting the abrasive grain by subjecting the crushed grain to an oxidizing atmosphere for from about 5 minutes to about 64 hours at a temperature of from about 1250°C to about 1450°C.
11. A process according to claim 10, wherein the TiO2 and alumina containing Na2O as the only oxide impurity present in an amount in excess of 0.1% by weight, are charged in amounts of 1.4 parts by weight and 98.5 parts by weight, respectively.
12. A process according to claim 10, wherein the alumina is tabular alumina having a maximum Na2O content of 0.15% by weight.
13. A process according to claim 10, wherein the alumina is calcined alumina.
14. A process according to claim 10, wherein the titania is electronic grade titania.
15. A process according to claim 10, wherein the carbon is calcined petroleum coke, present in an amount of from about 4 to about 7 times the theoretical amount necessary, based on the amount of TiO2 and Na2O added, to reduce the TiO2 and Na2O.
16. A process according to claim 10, wherein the carbon is graphite, present in an amount of from about 4 to about 7 times the theoretical amount necessary, based on the amount of TiO2 and Na2O added, to reduce the TiO2 and Na2O.
17. A process according to claim 10, wherein the electric arc is supplied by a single phase power supply hav-ing a voltage of about 80 volts and a power input of from about 100 to about 120 kilowatts.
18. A process according to claim 10, wherein the melted mixture is solidified by pouring into a cooling mold.
19. A process according to claim 18, wherein the melted mixture is poured into a water cooled steel pan to a depth of from about 2.5 to about 15 centimeters.
20. A process according to claim 19, wherein the melted mixture is poured to a depth of from about 2.5 to about 6 centimeters.
21. A process according to claim 18, wherein the melted mixture is poured into a solidification chamber containing steel spheres having a diameter ranging from about 5 to about 60 millimeters.
22. A process according to claim 21, wherein the steel spheres have a diameter of about 20 millimeters.
23. A process according to claim 18, wherein the length of pouring stream is minimized and the pour rate is maximized.
24. A process according to claim 10, wherein the oxidizing atmosphere is air.
25. A process according to claim 24, wherein the time of subjecting grain to oxidizing atmosphere ranges from about 5 to about 20 minutes.
26. A process according to claim 25, wherein the temperature to which the abrasive grain is subjected ranges from about 1300 to about 1350°C.
27. A process according to claim 26, wherein the time of subjecting grain to oxidizing atmosphere is about 10 minutes.
28. A process according to claim 27, wherein the temperature to which the abrasive grain is subjected is about 1300°C.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US05/691,817 US4111668A (en) | 1976-06-01 | 1976-06-01 | Fused aluminum oxide abrasive grain containing reduced titanium oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1074574A true CA1074574A (en) | 1980-04-01 |
Family
ID=24778101
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA277,176A Expired CA1074574A (en) | 1976-06-01 | 1977-04-27 | Fused aluminum oxide abrasive grain containing reduced titanium oxide |
Country Status (13)
| Country | Link |
|---|---|
| US (1) | US4111668A (en) |
| JP (1) | JPS6023715B2 (en) |
| AT (1) | AT362253B (en) |
| AU (1) | AU505412B2 (en) |
| BR (1) | BR7703484A (en) |
| CA (1) | CA1074574A (en) |
| CH (1) | CH622281A5 (en) |
| DE (1) | DE2723036A1 (en) |
| ES (1) | ES459159A1 (en) |
| FR (1) | FR2353617A1 (en) |
| GB (1) | GB1583184A (en) |
| SE (1) | SE435920B (en) |
| ZA (1) | ZA773241B (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AT358946B (en) * | 1979-02-07 | 1980-10-10 | Swarovski Tyrolit Schleif | METHOD FOR THE GOOD TREATMENT OF ABRASIVE GRAIN |
| DE3040992A1 (en) * | 1979-11-09 | 1981-05-27 | The Carborundum Co., Niagara Falls, N.Y. | ALUMINUM OXIDE GRINDING GRAIN AND METHOD FOR THE PRODUCTION THEREOF |
| US5143522B1 (en) * | 1979-11-09 | 1998-01-06 | Washington Mills Electro Miner | Abrasive products containing fused alumina zirconia and reduced titania |
| DE3026294A1 (en) * | 1980-07-11 | 1982-02-18 | Riedel-De Haen Ag, 3016 Seelze | CHLOROFLUOROFERRATE (II, III), METHOD FOR THE PRODUCTION THEREOF, ITS USE AND GRINDING WHEEL CONTAINING CHLOROFLUOROFERRATE (II, III) |
| JPS5973433A (en) * | 1982-09-23 | 1984-04-25 | エレクトロ・ミネラルズ（カナダ）インコーポレーテッド | Manufacture of low soda fused alumina |
| FI882662A (en) * | 1987-07-24 | 1989-01-25 | Lonza Ag | SLIPMEDEL. |
| AU589059B2 (en) * | 1987-12-16 | 1989-09-28 | Karl Reiling | Grinding body |
| YU32490A (en) * | 1989-03-13 | 1991-10-31 | Lonza Ag | Hydrophobic layered grinding particles |
| JP2599056Y2 (en) * | 1991-03-30 | 1999-08-30 | 三和テッキ株式会社 | Connection structure of wire connection bracket |
| JP2599057Y2 (en) * | 1991-03-30 | 1999-08-30 | 三和テッキ株式会社 | Connection structure of wire connection bracket |
| DE4306966C1 (en) * | 1992-10-19 | 1994-01-20 | Starck H C Gmbh Co Kg | Abrasive grain based on zirconium corundum, process for its production and its use |
| AU5789596A (en) * | 1996-05-03 | 1997-11-26 | Minnesota Mining And Manufacturing Company | Method and apparatus for manufacturing abrasive articles |
| WO1997042004A1 (en) * | 1996-05-03 | 1997-11-13 | Minnesota Mining And Manufacturing Company | Method of making a porous abrasive article |
| DE69627538T2 (en) * | 1996-05-03 | 2004-04-08 | Minnesota Mining And Manufacturing Company, St. Paul | NON-WOVEN ABRASIVES |
| US6451077B1 (en) | 2000-02-02 | 2002-09-17 | 3M Innovative Properties Company | Fused abrasive particles, abrasive articles, and methods of making and using the same |
| US6669749B1 (en) | 2000-02-02 | 2003-12-30 | 3M Innovative Properties Company | Fused abrasive particles, abrasive articles, and methods of making and using the same |
| US6592640B1 (en) | 2000-02-02 | 2003-07-15 | 3M Innovative Properties Company | Fused Al2O3-Y2O3 eutectic abrasive particles, abrasive articles, and methods of making and using the same |
| US6607570B1 (en) | 2000-02-02 | 2003-08-19 | 3M Innovative Properties Company | Fused Al2O3-rare earth oxide eutectic abrasive particles, abrasive articles, and methods of making and using the same |
| US6596041B2 (en) | 2000-02-02 | 2003-07-22 | 3M Innovative Properties Company | Fused AL2O3-MgO-rare earth oxide eutectic abrasive particles, abrasive articles, and methods of making and using the same |
| US6454822B1 (en) | 2000-07-19 | 2002-09-24 | 3M Innovative Properties Company | Fused aluminum oxycarbide/nitride-Al2O3·Y2O3 eutectic abrasive particles, abrasive articles, and methods of making and using the same |
| US6458731B1 (en) | 2000-07-19 | 2002-10-01 | 3M Innovative Properties Company | Fused aluminum oxycarbide/nitride-AL2O3.Y2O3 eutectic materials |
| US7384438B1 (en) | 2000-07-19 | 2008-06-10 | 3M Innovative Properties Company | Fused Al2O3-Y2O3-ZrO2 eutectic abrasive particles, abrasive articles, and methods of making and using the same |
| US6583080B1 (en) | 2000-07-19 | 2003-06-24 | 3M Innovative Properties Company | Fused aluminum oxycarbide/nitride-Al2O3·rare earth oxide eutectic materials |
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| CA2455902A1 (en) * | 2001-08-02 | 2003-12-18 | Anatoly Z. Rosenflanz | Alumina-yttria-zirconium oxide/hafnium oxide materials, and methods of making and using the same |
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| US7141522B2 (en) | 2003-09-18 | 2006-11-28 | 3M Innovative Properties Company | Ceramics comprising Al2O3, Y2O3, ZrO2 and/or HfO2, and Nb2O5 and/or Ta2O5 and methods of making the same |
| US7297171B2 (en) | 2003-09-18 | 2007-11-20 | 3M Innovative Properties Company | Methods of making ceramics comprising Al2O3, REO, ZrO2 and/or HfO2 and Nb205 and/or Ta2O5 |
| US7332453B2 (en) * | 2004-07-29 | 2008-02-19 | 3M Innovative Properties Company | Ceramics, and methods of making and using the same |
| US7497093B2 (en) * | 2004-07-29 | 2009-03-03 | 3M Innovative Properties Company | Method of making ceramic articles |
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| DE102011087147B4 (en) | 2011-11-25 | 2015-02-26 | C.A.R.R.D. Gmbh | Titanium oxide-containing aluminum oxide particles based on alumina melted in calcined alumina in an electric arc furnace, and a process for their production and their use |
| 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 |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR974041A (en) * | 1941-11-24 | 1951-02-16 | Melting process in an electric furnace or using any other source of sufficient heat, making it possible to obtain products based on alumina, silica and magnesia, which, after cooling, remain electrically conductive and new products resulting therefrom | |
| FR1100434A (en) * | 1953-03-23 | 1955-09-20 | Mountrose Schleifmittel Establ | Abrasives improvements |
| US3181939A (en) * | 1961-01-27 | 1965-05-04 | Norton Co | Fused alumina-zirconia abrasives |
| US3216794A (en) * | 1961-10-20 | 1965-11-09 | Norton Co | Process for producing crystalline alumina |
| US3428443A (en) * | 1965-07-26 | 1969-02-18 | Carborundum Co | Barrel finishing media |
| US3387957A (en) * | 1966-04-04 | 1968-06-11 | Carborundum Co | Microcrystalline sintered bauxite abrasive grain |
| US3491492A (en) * | 1968-01-15 | 1970-01-27 | Us Industries Inc | Method of making alumina abrasive grains |
| US3615308A (en) * | 1968-02-09 | 1971-10-26 | Norton Co | Crystalline abrasive alumina |
| US3928515A (en) * | 1971-06-15 | 1975-12-23 | Carborundum Co | Semicontinuous process for producing oxide refractory material having fine crystal structure |
| DE2420551B2 (en) * | 1974-04-27 | 1981-01-08 | Dynamit Nobel Ag, 5210 Troisdorf | Process for the production of grained abrasives from highly refractory inorganic hard materials |
-
1976
- 1976-06-01 US US05/691,817 patent/US4111668A/en not_active Expired - Lifetime
-
1977
- 1977-04-27 CA CA277,176A patent/CA1074574A/en not_active Expired
- 1977-05-21 DE DE19772723036 patent/DE2723036A1/en not_active Ceased
- 1977-05-26 ES ES459159A patent/ES459159A1/en not_active Expired
- 1977-05-26 GB GB22358/77A patent/GB1583184A/en not_active Expired
- 1977-05-30 ZA ZA00773241A patent/ZA773241B/en unknown
- 1977-05-30 BR BR7703484A patent/BR7703484A/en unknown
- 1977-05-30 JP JP52062295A patent/JPS6023715B2/en not_active Expired
- 1977-05-31 FR FR7716524A patent/FR2353617A1/en active Granted
- 1977-05-31 SE SE7706313A patent/SE435920B/en unknown
- 1977-05-31 CH CH664877A patent/CH622281A5/fr not_active IP Right Cessation
- 1977-05-31 AT AT382477A patent/AT362253B/en not_active IP Right Cessation
- 1977-05-31 AU AU25654/77A patent/AU505412B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| AT362253B (en) | 1981-04-27 |
| ES459159A1 (en) | 1978-04-16 |
| CH622281A5 (en) | 1981-03-31 |
| ATA382477A (en) | 1980-09-15 |
| SE435920B (en) | 1984-10-29 |
| FR2353617A1 (en) | 1977-12-30 |
| AU505412B2 (en) | 1979-11-22 |
| JPS52147393A (en) | 1977-12-07 |
| GB1583184A (en) | 1981-01-21 |
| BR7703484A (en) | 1978-03-14 |
| AU2565477A (en) | 1978-12-07 |
| JPS6023715B2 (en) | 1985-06-08 |
| ZA773241B (en) | 1978-04-26 |
| DE2723036A1 (en) | 1977-12-15 |
| US4111668A (en) | 1978-09-05 |
| SE7706313L (en) | 1977-12-02 |
| FR2353617B1 (en) | 1983-07-22 |
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