US3859407A - Method of manufacturing particles of uniform size and shape - Google Patents
Method of manufacturing particles of uniform size and shape Download PDFInfo
- Publication number
- US3859407A US3859407A US253186A US25318672A US3859407A US 3859407 A US3859407 A US 3859407A US 253186 A US253186 A US 253186A US 25318672 A US25318672 A US 25318672A US 3859407 A US3859407 A US 3859407A
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- 239000002245 particle Substances 0.000 title claims abstract description 121
- 238000004519 manufacturing process Methods 0.000 title description 12
- 239000000463 material Substances 0.000 claims abstract description 42
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 5
- 239000006061 abrasive grain Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 19
- 230000009969 flowable effect Effects 0.000 claims description 11
- 239000011195 cermet Substances 0.000 claims description 3
- 229920001187 thermosetting polymer Polymers 0.000 claims description 3
- 229920001169 thermoplastic Polymers 0.000 claims description 2
- 239000004416 thermosoftening plastic Substances 0.000 claims description 2
- 239000012815 thermoplastic material Substances 0.000 abstract description 5
- 238000001816 cooling Methods 0.000 abstract description 4
- 238000010304 firing Methods 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 3
- 239000012530 fluid Substances 0.000 abstract description 2
- 239000011521 glass Substances 0.000 description 6
- 230000001360 synchronised effect Effects 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 5
- 239000006060 molten glass Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 230000013011 mating Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000013618 particulate matter Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 230000002939 deleterious effect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- E—FIXED CONSTRUCTIONS
- E01—CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
- E01C—CONSTRUCTION OF, OR SURFACES FOR, ROADS, SPORTS GROUNDS, OR THE LIKE; MACHINES OR AUXILIARY TOOLS FOR CONSTRUCTION OR REPAIR
- E01C7/00—Coherent pavings made in situ
- E01C7/08—Coherent pavings made in situ made of road-metal and binders
- E01C7/085—Aggregate or filler materials therefor; Coloured reflecting or luminescent additives therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/22—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by pressing in moulds or between rollers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/004—Devices for shaping artificial aggregates from ceramic mixtures or from mixtures containing hydraulic binder
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
- B28B3/12—Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein one or more rollers exert pressure on the material
- B28B3/14—Producing shaped articles from the material by using presses; Presses specially adapted therefor wherein one or more rollers exert pressure on the material with co-operating pocketed rollers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/04—Making granules by dividing preformed material in the form of plates or sheets
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B11/00—Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing
- C03B11/06—Construction of plunger or mould
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B11/00—Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing
- C03B11/06—Construction of plunger or mould
- C03B11/08—Construction of plunger or mould for making solid articles, e.g. lenses
- C03B11/082—Construction of plunger or mould for making solid articles, e.g. lenses having profiled, patterned or microstructured surfaces
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B13/00—Rolling molten glass, i.e. where the molten glass is shaped by rolling
- C03B13/08—Rolling patterned sheets, e.g. sheets having a surface pattern
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/10—Forming beads
- C03B19/1005—Forming solid beads
- C03B19/1035—Forming solid beads by pressing
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/10—Forming beads
- C03B19/1005—Forming solid beads
- C03B19/104—Forming solid beads by rolling, e.g. using revolving cylinders, rotating discs, rolls
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2215/00—Press-moulding glass
- C03B2215/40—Product characteristics
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2215/00—Press-moulding glass
- C03B2215/40—Product characteristics
- C03B2215/41—Profiled surfaces
- C03B2215/412—Profiled surfaces fine structured, e.g. fresnel lenses, prismatic reflectors, other sharp-edged surface profiles
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2215/00—Press-moulding glass
- C03B2215/40—Product characteristics
- C03B2215/41—Profiled surfaces
- C03B2215/414—Arrays of products, e.g. lenses
Definitions
- ABSTRACT Plastically formable material which may be formed under pressure into desired shapes, is fed while in a fluid or plastically formable condition to a pair of cooperating surfaces which are relatively movable into compressive relationship with material disposed therebetween.
- the face of at least one of such surfaces is patterned with a plurality of juxtapositioned geometrical impressions of desired size and shape so as to form a ribbon or sheet of uniformly sized and shaped particles from the plastically formable material supplied to the cooperating surfaces.
- the uniform particles are initially joined together by thin web or edge portions which maintain the continuity of the newly formed particles within a sheet form.
- the ribbon of newly formed particles has become sufficiently rigid, such as through the cooling of a molten thermoplastic material or the drying or firing of a green ceramic material from which such ribbon may be formed, the ribbon may then be flexed in various directions to separate the particles along the edge or web portions, thus providing a plurality of individual particles having substantially uniform size and shape.
- the granules or particles manufactured by the present invention have utility in numerous fields including gripping elements for road surfaces and abrasive grains for use in bonded abrasive articles such as grinding wheels and snagging wheels, and coated abrasive articles such as abrasive papers and the like.
- gripping elements for road surfaces and abrasive grains for use in bonded abrasive articles such as grinding wheels and snagging wheels
- coated abrasive articles such as abrasive papers and the like.
- One of the problems that has plagued the industry in the manufacture of discrete particles for use as abrasive grains has been the inability to continually reproduce grains of the same size and shape. That is, it has been customary in the past to manufacture abrasive grains by crushing abrasive type material into granular form.
- U.S. Pat. No. 3,481,723 illustrates a method of producing shaped abrasive grains by extruding predetermined lengths of a green ceramic mixture which is then sintered to form hard abrasive grains.
- the shape of such grains is severely limited to a pre-shaped cylindrical or prismatic configuration, with the only variable crosssection lying in a plane perpendicular to the axis of extrusion. Therefore, although the extruded sintered abrasive grains were an improvement over the randomly crushed grains, they have not been entirely satisfactory since variable three-dimensional geometric solids are not obtainable and the manufacturing process is not particularly economical.
- the present invention not only obviates the problem of repeatably producing uniform particles of virtually identical size and shape, but also provides a simplified continuous or repeatable process for rapidly and economically producing such particles in mass production.
- the present invention sets forth a completely new concept in the manufacture of particulate matter having uniform size and shape from a flowable plastically formable material.
- the present invention includes the flowing of plastically formable material to a pair of cooperating forming members having one or more of the cooperating surfaces thereof engraved or contoured with recesses or patterns of desired size and shape. Accordingly, the cooperating members produce a plurality of uniform particles of substantially identical size and shape which are joined together along adjacent connecting edge portions by means of a thin web portion.
- Any flowable plastically formable material may be supplied to the cooperating members including thermoplastic materials such as basalts and molten vitreous materials, as well as thixotropic and thermosetting materials such as ceramic batches, wherein all such materials have the property of being able to flow and be plastically formed during the application of forming pressure, while also being able to become sufficiently rigid immediately thereafter so as to maintain structural integrity. That is, when the particles are formed of a thermoplastic material, the ribbon of newly formed particles is cooled and solidified immediately thereafter in order to provide sufficient rigidity so as to maintain the structural integrity of the newly formed particles, whereas when such ribbon is formed of a ceramic batch, it may be dried or fired in order to obtain the necessary rigidity.
- thermoplastic materials such as basalts and molten vitreous materials
- thixotropic and thermosetting materials such as ceramic batches
- the cooperating forming members may be either a pair of cooperating forming rollers or a mold and plunger set. That is, the particles may either be roll-formed or press-formed depending upon the particular forming device utilized, however, in both instances the forming of the plastically formable material is accomplished through a pressing force exerted between a pair of forming members having one or more cooperating surfaces thereof contoured with patterns for forming the particles of desired size and shape.
- Roll-forming has the advantage of providing a continuous forming process
- press-forming by means of a mold and plunger has the advantage of greater flexibility in providing lower volume speciality items.
- the resulting particles which extend solely from one surface of the ribbon with the opposite surface being flat, such as may be utilized with coated abrasive sheets; or the particles may project outwardly in staggered relation from opposite sides of the resulting sheet; or finally, the recesses in the opposed faces may be mated or aligned and synchronized so that the resulting particles have opposed apexes projecting equally distant on opposite sides of the ribbon from a thin web-like plane bisecting the axis between such apexes.
- the recesses or impressions formed in the cooperating surfaces are of a desired uniform size and shape, the resulting particles formed thereby are also virtually identical in both size and configuration, thus providing a theoretical selection.
- the newly formed particles may be conveniently conveyed or transported in ribbon form for further processing as may be desired, and the plurality of particles making up the ribbon may, after becoming sufficiently rigidified to prevent deformation, then be separated or liberated therefrom in individual form by various means such as a pair of soft, off-set rolls.
- the rolls cause the substantially rigid sheet or ribbon of particles to flex in various directions out of the plane of the sheet, thus liberating or separating the particles along the edge or web portions from the sheet as individual grains of uniform size and shape which may then be conveniently collected for bulk packaging. It will be apparent, however, that the individual particles may be liberated from the ribbon either before or after any additional treatment, such as metallizing, is undertaken.
- FIG. 1 is a somewhat schematic perspective view illustrating the process and apparatus of the present invention for continuously forming particles of substantially identical size and shape.
- FIG. la is a sectional view illustrating a further embodiment.
- FIG. 2 is an elevational view in section through the bite of a pair of cooperating rollers.
- FIG. 3 is a greatly enlarged fragmental view in plan of a plurality of particles in ribbon form produced by the rollers of FIG. 2.
- FIG. 4 is a greatly enlarged fragmental view of a plurality of particles after they have been liberated or separated from the ribbon of particles shown in FIG. 3.
- FIGS. 5a, 6a, 7a, 8a, 9a and 10a illustrate various shapes of particles in ribbon form which may be produced by the present invention, whereas corresponding FIGS. 5b, 6b, 7b, 8b, 9b and 10b illustrate the shape of the individual particles after they have been separated or liberated from their corresponding ribbon.
- the ribbon R is shown as being discontinuous between conveyor rollers 18 to indicate that additional processing such as solidifying, drying, firing and metallizing may be imparted to the ribbon as desired prior to the liberating or separating of the various particles therefrom into their individual state.
- additional processing such as solidifying, drying, firing and metallizing
- the newly formed ribbon R if of a siliceous vitreous material, may be subjected to a metallizing treatment such as by contacting it with molten aluminum as described in US. Pat. No. 2,702,750, so as to form cermet particles which are especially suited for heavy-duty abrasive grain application.
- the recessed or engraved patterned surface may be formed in either or both of the cooperating rollers 10, 12 as desired.
- the recessed or engraved pattern is formed in the surface of only one roller and the opposed surface of the other cooperating roller is smooth, a plurality of particles are formed within the resulting ribbon having a flat or planar back surface, with the particles projecting outwardly only from one side of such ribbon and being joined together along adjacent edge portions thereof.
- both of the operating surfaces l4, 16 of the cooperating forming rolls l0, 12 may be provided with desired impressions to provide a specific pattern on both sides of a ribbon of material which passes through the bite of such rollers.
- the impressions made in the roller surfaces are uniform with respect to one another and may be of any desired size and shape such as tetrahedra, cubes, octahedra and other geometric shapes.
- the particles formed by the recessed surfaces are initially joined together in ribbon form, either along common edge portions or by means of a narrow thin web of vitreous material, with the exact manner in which the particles are joined being dependent upon the shape being produced.
- the recesses or impressions in each such surface may be staggered or off-set as illustrated in the embodiment shown in FIG. 2, or the impressions on the surfaces may be synchronized by the speed of rotation of the rollers so that the patterns on opposing rollers are matched when in contact with the plastically formable material at the bite of the rollers.
- the forming members shown as plunger 10a and mold 12a are provided with cooperating surfaces having mating or matched impressions so that the patterns cooperate to form a ribbon of particles within the mold which extend outwardly from opposite sides of the ribbon per se.
- the resultant particles may be symmetrical about a plane perpendicularly bisecting an axis passing through a pair of opposed apexes formed by each such particle.
- adjacent particles may be connected to one another in ribbon form either by connecting edge portions or by a small connecting web portion, however, in either case the particles may be liberated from the ribbon form to their separate state by means of a pair of off-set flexing rolls or the like which permit the connected particles to break apart from the ribbon while maintaining their initially formed individual integrity.
- any size of particle above 0.01 inches may be formed with the present invention, for the purpose of manufacturing abrasive grains we prefer to form articles having an altitude, or apex to apex distance, of between about 0.028 inches and 0.157 inches. It will be apparent that the upper size limit of particle manufacture will be limited only by the pressing capacity of the cooperating surfaces, whereas the lower limit of about 0.01 inches is dictated by the minimum thickness of the resulting web which would be sufficient to maintain the integrity of the ribbon.
- the individual geometric shapes of the particular particles may be liberated from the rigidified ribbon or sheet by providing a sufficient deflection of the ribbon to cause a brittle fracture along the thinnest portions thereof, such as the common edges of the particle shapes or the thin web of vitreous material between such shapes.
- the liberated particles of geometric shapes are then collected and further processed as dictated by their end use.
- the forming rollers 110, 112 are provided with recessed or engraved pattern surfaces 114, 116 which are staggered or off-set with one another at the bite 118 of the rollers.
- Each of the patterned surfaces 114, 116 is provided with a plurality of pyramidal or tetrahedral shaped recesses of equal size and shape.
- the plastically formable material G such as molten glass, which is fed to the forming rollers 110, 112, is formed into a ribbon R having a plurality of off-set tetrahedral or pyramidal particles P extending outwardly from both sides thereof. As shown in FIG.
- the pyramidal particles P extending outwardly from one side of the ribbon R are bound together along connecting edges 120 of the flats or bottoms 122 of pyramidal particles P extending outwardly from the opposite side of the ribbon.
- the individual particles P after being liberated from the ribbon R and falling into the container 22, are all of the same size and shape as originally formed by the cavities or recesses of the forming rollers.
- FIGS. 5a through b which illustrate some of the various forms of ribbons and particles which may be produced by the present invention
- the ribbons shown in FIGS. 5a, 6a, 7a and 8a all have a flat or planar back or bottom surface, such as would be produced when only one roll or mold surface is provided with a recessed or engraved pattern.
- the ribbon 50 of FIG. 5a is formed of a plurality of particles 51, shown in FIG. 5b, having the appearance of a slightly rounded cube or frustum.
- the web or connecting edge portion of the particles 51 is shown at 120.
- ribbon 100 produces particles 101, each of which has a pair of symmetrical shapes, similar to particle 51, extending outwardly on opposite sides of the ribbon from a plane perpendicularly bisecting an axis extending between opposed apexes of the particle 101.
- the connecting edge or web portions which lie in the bisecting plane are shown at 120.
- Ribbon 60, of FIG. 6a produces a plurality of pyramids 61 having a square base and four triangular sides converging at an apex. If a second roller, having a patterned recess similar to that on the first roller forming particle 61, were synchronized with such first roller, a particle projecting outwardly from opposite sides of the ribbon and having an octrahedral configuration would be formed.
- FIG. 7a illustrates a ribbon for forming a multi-surfaced particle 71 having numerous edges which are useful when the particle is used as a cutting grain.
- FIG. 8a illustrates a ribbon which produces particles 81 having an eight-sided configuration.
- ribbons 50, 60, 70 and 80 which are provided with a flat or planar back surface, may be utilized in the as-produced ribbon form, after being suitably treated, by providing the same with backing sheets so as to form coated abrasive articles.
- FIG. 9a illustrates a ribbon for producing particles 91 having a hexahedral configuration.
- Such configuration would be formed by rollers 110, 112, when the speed thereof is adjusted so that the impressed or recessed portions 114, 116 are synchronized and cooper ate with one another as they pass through the bite 118 of the rollers.
- the mating surfaces of plunger 10a and mold 1211 could produce the hexahedral particle configuration of FIGS. 90 and 9b.
- particle 91 is characterized by a pair of opposed pyramids projecting outwardly from opposite sides of the ribbon 90 such that the connecting web 120 or plane of the ribbon 90 bisects and axis extending between opposed apexes 92 of the hexahedral configuration of the shaped particle 91.
- the present invention permits a highly controlled geometric shape of the particle is of particular significance when such particle is used as an abrasive grain. That is, improved abrasive performance can be achieved by controlling the shape to maximize grain sharpness and grain toughness. Also, the shape can be designed to supply anchors for the resin or other bond utilized to hold the grains on a grinding or snagging wheel and thereby increase the strength and life of such a wheel. Further, the shape may be optimized to increase the particle packing of the grains and thus increase the volume of grains per wheel. Finally, the present process allows for very accurate control of the particle size distribution of the grains produced, and therefor permits the manufacture of highly reproducible abrasive products from such grains.
- any desired geometric shape of particle may be continuously or intermittantly reproduced either in a single patterned surface or in cooperating patterned surfaces, and such particles may be formed of virtually any desired plastically formable material which becomes rigid and sets-up after forming, such as by firing or cooling.
- the particles are formed from green ceramic material or thermoplastic materials, such as basalts or siliceous glass compositions, with the latter progiding a basis for transforming the particles into cermets by known metallizing processes.
- Such metallizing processes are described in US. Pat. No. 2,702,750, however, we prefer to subject the newly formed siliceous particles into contact with molten aluminum at about 700C for about 2 Va to 10 hours, for No. 20 to No. 6 grit sizes, respectively.
- operating parameters may vary over wide limits depending upon the material being produced, the following specific example is given merely for purposes of illustration.
- a 17.6% MgO-29.7% Al O -9.1% B O -43.6% SiO glass was melted at l,650C and poured at about l,400C between a pair of cooperating water cooled stainless steel forming rolls.
- Each of the rolls was provided with an engraved or recessed patterned surface in the form of one half of an octrahedra] impression, and the rolls were then synchronized so that the patterns on opposing rolls were matched when in contact with the molten glass at the bite thereof.
- the rolls were rotated at approximately 28 RPM and spaced about 0.005 inches apart.
- the formed glass ribbon was pulled vertically downwardly from the rolls and contained small glass octrahedra measuring 0.069 inches from point to point along an axis extending between opposed apexes thereof.
- the octrahedra were separated by a thin web of glass which laid within a plane bisecting the axis extending between the apexes. On cooling, theribbon was easily broken'to liberate the small glass octrahedra which were then collected for further treatment.
- a method of continuously forming particles of uniform size and shape from flowable batch material which comprises:
- a method of continuously forming uniform abrasive grains of desired size and shape from flowable thermoplastic vitreous or thermosetting ceramic material comprising:
- a method of continuously forming uniform abrasive grains of desired size and shape from flowable siliceous material comprising:
Abstract
Plastically formable material, which may be formed under pressure into desired shapes, is fed while in a fluid or plastically formable condition to a pair of cooperating surfaces which are relatively movable into compressive relationship with material disposed therebetween. The face of at least one of such surfaces is patterned with a plurality of juxtapositioned geometrical impressions of desired size and shape so as to form a ribbon or sheet of uniformly sized and shaped particles from the plastically formable material supplied to the cooperating surfaces. The uniform particles are initially joined together by thin web or edge portions which maintain the continuity of the newly formed particles within a sheet form. However, after the ribbon of newly formed particles has become sufficiently rigid, such as through the cooling of a molten thermoplastic material or the drying or firing of a green ceramic material from which such ribbon may be formed, the ribbon may then be flexed in various directions to separate the particles along the edge or web portions, thus providing a plurality of individual particles having substantially uniform size and shape.
Description
United States Patent [191 Blanding et al.
1 Jan. 7, 1975 METHOD OF MANUFACTURING PARTICLES OF UNIFORM SIZE AND SHAPE [75] Inventors: Wendell S. Blanding, Painted Post; Jack A. Brothers, Corning, both of [73] Assignee: Corning Glass Works, Corning,
[22] Filed: May 15, 1972 [21] Appl. No.: 253,186
[52] US. Cl 264/62, 51/295, 51/307, 51/309, 51/DIG. 30, 65/97, 65/101, 264/56, 264/133, 264/140, 264/175, 425/116 [51] Int. Cl. C04b 41/14, C04b 41/24 [58] Field of Search; 264/67, 140, 144, 214, 264/332, 175, 133; 65/87, 93, 97, 101, 245; 425/115, 116; 51/295, 307, 309, DIG. 30
Great Britain 264/144 Great Britain 65/101 [5 7] ABSTRACT Plastically formable material, which may be formed under pressure into desired shapes, is fed while in a fluid or plastically formable condition to a pair of cooperating surfaces which are relatively movable into compressive relationship with material disposed therebetween. The face of at least one of such surfaces is patterned with a plurality of juxtapositioned geometrical impressions of desired size and shape so as to form a ribbon or sheet of uniformly sized and shaped particles from the plastically formable material supplied to the cooperating surfaces. The uniform particles are initially joined together by thin web or edge portions which maintain the continuity of the newly formed particles within a sheet form. However, after the ribbon of newly formed particles has become sufficiently rigid, such as through the cooling of a molten thermoplastic material or the drying or firing of a green ceramic material from which such ribbon may be formed, the ribbon may then be flexed in various directions to separate the particles along the edge or web portions, thus providing a plurality of individual particles having substantially uniform size and shape.
3 Claims, 17 Drawing Figures PATENTED A 71975 sum 1 BF 3 PATENTED (I975 3,859,407
SHEET 2 OF 3 QQ A? if R FA%AWY?AWAWYZ TWWY wm aw METHOD OF MANUFACTURING PARTICLES OF UNIFORM SIZE AND SHAPE BACKGROUND OF THE INVENTION The present invention resides in the field of discrete particle manufacture, and particularly is concerned with the problem of repeatably forming particles having virtually identical size and shape.
The granules or particles manufactured by the present invention have utility in numerous fields including gripping elements for road surfaces and abrasive grains for use in bonded abrasive articles such as grinding wheels and snagging wheels, and coated abrasive articles such as abrasive papers and the like. One of the problems that has plagued the industry in the manufacture of discrete particles for use as abrasive grains has been the inability to continually reproduce grains of the same size and shape. That is, it has been customary in the past to manufacture abrasive grains by crushing abrasive type material into granular form. However, in the case of heavy duty abrasive grits, usually less than 50% of the total material is recovered in a usable size range, with the majority of the material being crushed into useless fines. Further, that material which is usable must then be classified into standard grain sizes. However, since the crushing process cannot be accurately controlled, the shape of the grains even within a particular classification will vary materially, thus producing grains with dissimilar cutting rates and variable useful lives, thereby resulting in less than optimal efficiencies. The shape of crushed abrasive particles can be improved somewhat by mulling, however such process is not only costly but results in even lower recoveries.
U.S. Pat. No. 3,481,723 illustrates a method of producing shaped abrasive grains by extruding predetermined lengths of a green ceramic mixture which is then sintered to form hard abrasive grains. However, due to the extrusion forming thereof, the shape of such grains is severely limited to a pre-shaped cylindrical or prismatic configuration, with the only variable crosssection lying in a plane perpendicular to the axis of extrusion. Therefore, although the extruded sintered abrasive grains were an improvement over the randomly crushed grains, they have not been entirely satisfactory since variable three-dimensional geometric solids are not obtainable and the manufacturing process is not particularly economical.
The present invention not only obviates the problem of repeatably producing uniform particles of virtually identical size and shape, but also provides a simplified continuous or repeatable process for rapidly and economically producing such particles in mass production.
SUMMARY OF THE INVENTION The present invention sets forth a completely new concept in the manufacture of particulate matter having uniform size and shape from a flowable plastically formable material. In its simplest form, the present invention includes the flowing of plastically formable material to a pair of cooperating forming members having one or more of the cooperating surfaces thereof engraved or contoured with recesses or patterns of desired size and shape. Accordingly, the cooperating members produce a plurality of uniform particles of substantially identical size and shape which are joined together along adjacent connecting edge portions by means of a thin web portion.
Any flowable plastically formable material may be supplied to the cooperating members including thermoplastic materials such as basalts and molten vitreous materials, as well as thixotropic and thermosetting materials such as ceramic batches, wherein all such materials have the property of being able to flow and be plastically formed during the application of forming pressure, while also being able to become sufficiently rigid immediately thereafter so as to maintain structural integrity. That is, when the particles are formed of a thermoplastic material, the ribbon of newly formed particles is cooled and solidified immediately thereafter in order to provide sufficient rigidity so as to maintain the structural integrity of the newly formed particles, whereas when such ribbon is formed of a ceramic batch, it may be dried or fired in order to obtain the necessary rigidity.
Depending upon the particular application to which the particles are to be utilized, the cooperating forming members may be either a pair of cooperating forming rollers or a mold and plunger set. That is, the particles may either be roll-formed or press-formed depending upon the particular forming device utilized, however, in both instances the forming of the plastically formable material is accomplished through a pressing force exerted between a pair of forming members having one or more cooperating surfaces thereof contoured with patterns for forming the particles of desired size and shape. Roll-forming has the advantage of providing a continuous forming process, whereas press-forming by means of a mold and plunger has the advantage of greater flexibility in providing lower volume speciality items.
In view of the fact that the basic forming operation of the present invention, which includes the exertion of pressure by two cooperating surfaces on plastically formable material to product particles of a given size and shape, may be accomplished by either roll-forming or linear press-forming, the invention will be described in particular only with respect to roll-forming, as the similarities between the two processes will be readily appreciated by those skilled in the art. Depending upon the surface patterning and the orientation of the cooperating members, it is possible to form particles which extend solely from one surface of the ribbon with the opposite surface being flat, such as may be utilized with coated abrasive sheets; or the particles may project outwardly in staggered relation from opposite sides of the resulting sheet; or finally, the recesses in the opposed faces may be mated or aligned and synchronized so that the resulting particles have opposed apexes projecting equally distant on opposite sides of the ribbon from a thin web-like plane bisecting the axis between such apexes. In all cases, however, since the recesses or impressions formed in the cooperating surfaces are of a desired uniform size and shape, the resulting particles formed thereby are also virtually identical in both size and configuration, thus providing a theoretical selection.
The newly formed particles may be conveniently conveyed or transported in ribbon form for further processing as may be desired, and the plurality of particles making up the ribbon may, after becoming sufficiently rigidified to prevent deformation, then be separated or liberated therefrom in individual form by various means such as a pair of soft, off-set rolls. The rolls cause the substantially rigid sheet or ribbon of particles to flex in various directions out of the plane of the sheet, thus liberating or separating the particles along the edge or web portions from the sheet as individual grains of uniform size and shape which may then be conveniently collected for bulk packaging. It will be apparent, however, that the individual particles may be liberated from the ribbon either before or after any additional treatment, such as metallizing, is undertaken.
It thus has been an object of the present invention to obviate the uneconomical and virtually uncontrollable prior art processes of forming particulate matter usable as abrasive grains or highway traction particles, by providing an improved process of forming, such as by continuously rolling, a plurality of interconnected particles of like size and shape in ribbon form from plastically formable material such as green ceramic or molten vitreous material, with the ribbon of connected particles, after rigidification, being subsequently separable into uniform individual particles.
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a somewhat schematic perspective view illustrating the process and apparatus of the present invention for continuously forming particles of substantially identical size and shape.
FIG. la is a sectional view illustrating a further embodiment.
FIG. 2 is an elevational view in section through the bite of a pair of cooperating rollers.
FIG. 3 is a greatly enlarged fragmental view in plan of a plurality of particles in ribbon form produced by the rollers of FIG. 2. i
FIG. 4 is a greatly enlarged fragmental view of a plurality of particles after they have been liberated or separated from the ribbon of particles shown in FIG. 3.
FIGS. 5a, 6a, 7a, 8a, 9a and 10a illustrate various shapes of particles in ribbon form which may be produced by the present invention, whereas corresponding FIGS. 5b, 6b, 7b, 8b, 9b and 10b illustrate the shape of the individual particles after they have been separated or liberated from their corresponding ribbon.
DESCRIPTION OF THE PREFERRED EMBODIMENTS cessed patterned surfaces 14, 16, roll-forms a flow of plastically formable material G, such as green ceramic batch or molten glass or basalts, into a continuous ribbon R of interconnected particles P. The rollers are rotatable about parallel longitudinal axes toward one another as shown by the arrows, so that the flowable material G supplied thereto is roll-formed as it passes through the bite. As shown, the ribbon may be transferred along conveyor rollers 18 to a pair of soft, off-set flexing rolls 20 which distort and flex the now rigidified ribbon R in various directions out of its natural plane and thereby liberate the connected particles P from the ribbon so they may fall as separate individual particles P and be collected in a container 22. The ribbon R is shown as being discontinuous between conveyor rollers 18 to indicate that additional processing such as solidifying, drying, firing and metallizing may be imparted to the ribbon as desired prior to the liberating or separating of the various particles therefrom into their individual state. For example, the newly formed ribbon R, if of a siliceous vitreous material, may be subjected to a metallizing treatment such as by contacting it with molten aluminum as described in US. Pat. No. 2,702,750, so as to form cermet particles which are especially suited for heavy-duty abrasive grain application.
The recessed or engraved patterned surface may be formed in either or both of the cooperating rollers 10, 12 as desired. When the recessed or engraved pattern is formed in the surface of only one roller and the opposed surface of the other cooperating roller is smooth, a plurality of particles are formed within the resulting ribbon having a flat or planar back surface, with the particles projecting outwardly only from one side of such ribbon and being joined together along adjacent edge portions thereof. When such a ribbon is formed having a flat or planar back surface, it may be desirable, after appropriate treatment, to utilize the particles in ribbon form in a coated abrasive article by applying a backing thereto, without requiring the separat ing or liberating of the individual particles from the ribbon.
As shown in the schematic illustration of FIG. 1, both of the operating surfaces l4, 16 of the cooperating forming rolls l0, 12 may be provided with desired impressions to provide a specific pattern on both sides of a ribbon of material which passes through the bite of such rollers. The impressions made in the roller surfaces are uniform with respect to one another and may be of any desired size and shape such as tetrahedra, cubes, octahedra and other geometric shapes. As previously pointed out, the particles formed by the recessed surfaces are initially joined together in ribbon form, either along common edge portions or by means of a narrow thin web of vitreous material, with the exact manner in which the particles are joined being dependent upon the shape being produced.
When both of the cooperating rollers are provided with engraved surfaces, the recesses or impressions in each such surface may be staggered or off-set as illustrated in the embodiment shown in FIG. 2, or the impressions on the surfaces may be synchronized by the speed of rotation of the rollers so that the patterns on opposing rollers are matched when in contact with the plastically formable material at the bite of the rollers. Similarly, as illustrated in FIG. la, the forming members shown as plunger 10a and mold 12a are provided with cooperating surfaces having mating or matched impressions so that the patterns cooperate to form a ribbon of particles within the mold which extend outwardly from opposite sides of the ribbon per se. Accordingly, the resultant particles may be symmetrical about a plane perpendicularly bisecting an axis passing through a pair of opposed apexes formed by each such particle. Whether the opposed patterns on the forming members are mated in synchronized relation or not, adjacent particles may be connected to one another in ribbon form either by connecting edge portions or by a small connecting web portion, however, in either case the particles may be liberated from the ribbon form to their separate state by means of a pair of off-set flexing rolls or the like which permit the connected particles to break apart from the ribbon while maintaining their initially formed individual integrity. That is, since the flexing rolls do not affect the size or shape of the individual particles per se, but merely separates one from another, it is possible to continuously and repeatably produce particles of a given size and shape with about 95-100% selection, since there is no crushing or deleterious deformation of the particles as was occasioned in the prior art processes.
Although virtually any size of particle above 0.01 inches may be formed with the present invention, for the purpose of manufacturing abrasive grains we prefer to form articles having an altitude, or apex to apex distance, of between about 0.028 inches and 0.157 inches. It will be apparent that the upper size limit of particle manufacture will be limited only by the pressing capacity of the cooperating surfaces, whereas the lower limit of about 0.01 inches is dictated by the minimum thickness of the resulting web which would be sufficient to maintain the integrity of the ribbon. As previously mentioned, the individual geometric shapes of the particular particles may be liberated from the rigidified ribbon or sheet by providing a sufficient deflection of the ribbon to cause a brittle fracture along the thinnest portions thereof, such as the common edges of the particle shapes or the thin web of vitreous material between such shapes. The liberated particles of geometric shapes are then collected and further processed as dictated by their end use.
Referring now to the embodiment shown in FIG. 2, the forming rollers 110, 112 are provided with recessed or engraved pattern surfaces 114, 116 which are staggered or off-set with one another at the bite 118 of the rollers. Each of the patterned surfaces 114, 116 is provided with a plurality of pyramidal or tetrahedral shaped recesses of equal size and shape. Accordingly, the plastically formable material G, such as molten glass, which is fed to the forming rollers 110, 112, is formed into a ribbon R having a plurality of off-set tetrahedral or pyramidal particles P extending outwardly from both sides thereof. As shown in FIG. 3, the pyramidal particles P extending outwardly from one side of the ribbon R are bound together along connecting edges 120 of the flats or bottoms 122 of pyramidal particles P extending outwardly from the opposite side of the ribbon. As shown in FIG. 4, the individual particles P, after being liberated from the ribbon R and falling into the container 22, are all of the same size and shape as originally formed by the cavities or recesses of the forming rollers.
Referring now to FIGS. 5a through b which illustrate some of the various forms of ribbons and particles which may be produced by the present invention, it will be noted that the ribbons shown in FIGS. 5a, 6a, 7a and 8a all have a flat or planar back or bottom surface, such as would be produced when only one roll or mold surface is provided with a recessed or engraved pattern. The ribbon 50 of FIG. 5a is formed of a plurality of particles 51, shown in FIG. 5b, having the appearance of a slightly rounded cube or frustum. The web or connecting edge portion of the particles 51 is shown at 120. It should be further noted, that the ribbon 100 shown in FIG. 10a and the particle 101 of FIG. 10b formed therefrom, may be produced by synchronizing two forming rollers having the same surface pattern which forms ribbon 50 of FIG. 5a. That is, ribbon 100 produces particles 101, each of which has a pair of symmetrical shapes, similar to particle 51, extending outwardly on opposite sides of the ribbon from a plane perpendicularly bisecting an axis extending between opposed apexes of the particle 101. The connecting edge or web portions which lie in the bisecting plane are shown at 120.
FIG. 9a illustrates a ribbon for producing particles 91 having a hexahedral configuration. Such configuration would be formed by rollers 110, 112, when the speed thereof is adjusted so that the impressed or recessed portions 114, 116 are synchronized and cooper ate with one another as they pass through the bite 118 of the rollers. Also the mating surfaces of plunger 10a and mold 1211 could produce the hexahedral particle configuration of FIGS. 90 and 9b. Accordingly, particle 91 is characterized by a pair of opposed pyramids projecting outwardly from opposite sides of the ribbon 90 such that the connecting web 120 or plane of the ribbon 90 bisects and axis extending between opposed apexes 92 of the hexahedral configuration of the shaped particle 91.
The fact that the present invention permits a highly controlled geometric shape of the particle is of particular significance when such particle is used as an abrasive grain. That is, improved abrasive performance can be achieved by controlling the shape to maximize grain sharpness and grain toughness. Also, the shape can be designed to supply anchors for the resin or other bond utilized to hold the grains on a grinding or snagging wheel and thereby increase the strength and life of such a wheel. Further, the shape may be optimized to increase the particle packing of the grains and thus increase the volume of grains per wheel. Finally, the present process allows for very accurate control of the particle size distribution of the grains produced, and therefor permits the manufacture of highly reproducible abrasive products from such grains.
From the foregoing it will be appreciated that virtually any desired geometric shape of particle may be continuously or intermittantly reproduced either in a single patterned surface or in cooperating patterned surfaces, and such particles may be formed of virtually any desired plastically formable material which becomes rigid and sets-up after forming, such as by firing or cooling. Preferably, the particles are formed from green ceramic material or thermoplastic materials, such as basalts or siliceous glass compositions, with the latter progiding a basis for transforming the particles into cermets by known metallizing processes. Such metallizing processes are described in US. Pat. No. 2,702,750, however, we prefer to subject the newly formed siliceous particles into contact with molten aluminum at about 700C for about 2 Va to 10 hours, for No. 20 to No. 6 grit sizes, respectively. Although it will be appreciated that operating parameters may vary over wide limits depending upon the material being produced, the following specific example is given merely for purposes of illustration.
A 17.6% MgO-29.7% Al O -9.1% B O -43.6% SiO glass was melted at l,650C and poured at about l,400C between a pair of cooperating water cooled stainless steel forming rolls. Each of the rolls was provided with an engraved or recessed patterned surface in the form of one half of an octrahedra] impression, and the rolls were then synchronized so that the patterns on opposing rolls were matched when in contact with the molten glass at the bite thereof. The rolls were rotated at approximately 28 RPM and spaced about 0.005 inches apart. The formed glass ribbon was pulled vertically downwardly from the rolls and contained small glass octrahedra measuring 0.069 inches from point to point along an axis extending between opposed apexes thereof. The octrahedra were separated by a thin web of glass which laid within a plane bisecting the axis extending between the apexes. On cooling, theribbon was easily broken'to liberate the small glass octrahedra which were then collected for further treatment.
Although we have disclosed the now preferred embodiments of our invention, it will be apparent to those skilled in the art that various changes and modifications may be made thereto without departing from the spirit and scope thereof as defined in the appended claims.
We claim:
l. A method of continuously forming particles of uniform size and shape from flowable batch material which comprises:
a. providing "a pair of cooperating forming rollers,
b. providing a patterned surface having a plurality of individual uniform recesses of desired size and shape across and about an operating surface of at least one of said cooperating rollers,
c. supplying a flow of said flowable batch material to the bite of said cooperating rollers,
d. roll-forming between said pair of cooperating rollers a longitudinally continuous ribbon of particles of uniform size and shape connected together along adjacent edge portions by a web portion extending the width of said patterned surface, and
e. flexing the ribbon between a pair of off-set rolls out of the plane of the ribbon to liberate the connected particles therefrom into a plurality of individual separated particles of the same uniform size and shape as initially produced in ribbon form.
2. A method of continuously forming uniform abrasive grains of desired size and shape from flowable thermoplastic vitreous or thermosetting ceramic material comprising:
a. providing a pair of cooperating forming rollers rotatable about parallel longitudinal axes,
b. providing patterned particle-forming surface portions on opposed surfaces of said forming rollers,
c. supplying a flow of said material to the bite of said cooperating rollers,
d. synchronizing said pair of cooperating rollers so that opposed patterned surface portions cooperate with one another,
e. roll-forming between said cooperating rollers a longitudinally continuous ribbon of a plurality of adjacent particles connected together by means of a continuous connecting thin web portion extending across the width of the patterned surface portions and having opposed apexes which extend outwardly from opposite sides of the ribbon such that the plane of said web portion perpendicularly bisects an axis extending between a pair of opposed apexes, and
f. flexing said ribbon between a pair of off-set rolls in various directions out of the plane of the ribbon to separate the newly formed abrasive particles therefrom along adjacent edge portions into individual particles of desired uniform size and shape for use as abrasive grains.
3. A method of continuously forming uniform abrasive grains of desired size and shape from flowable siliceous material comprising:
a. providing a pair of cooperating forming rollers rotatable about parallel longitudinal axes,
b. providing patterned particle-forming surface portions on opposed surfaces of said forming rollers,
c. supplying a flow of siliceous material to the bite of said cooperating rollers,
d. roll-forming between said cooperating rollers a longitudinally continuous ribbon of particles of uniform size and shape connected together along adjacent edge portions by interconnected web portions,
e. metallizing said particles of siliceous material while in said ribbon form to form cermet abrasive grains, and
f. flexing said ribbon of abrasive grains between a pair of off-set rolls in various directions out of the plane of the ribbon to separate the newly formed abrasive grains therefrom along adjacent edge portions into individual abrasive particles of desired uniform size and shape.
Claims (3)
1. A METHOD OF CONTINUOUSLY FORMING PARTICLES OF UNIFORM SIZE AND SHAPE FROM FLOWABLE BATCH MATERIAL WHICH COMPRISES: A. PROVIDING A PAIR OF COOPERATING FORMING ROLLERS, B. PROVIDING A PATTERNED SURFACE HAVING PLURALITY OF INDIVIDUAL UNIFORM RECESSES OF DESIRED SIZE AND SHAPE ACROSS AND ABOUT AN OPERATING SURFACE OF AT LEAST ONE OF SAID COOPERATIONG ROLLERS, C. SUPPLYING A FLOW OF SAID FLOWABLE BATCH MATERIAL TO THE BITE OF SAID COOPERATING ROLLERS, D. ROLL-FORMING BETWEEN SAID PAIR OF COOPERATING ROLLERS A LONGITUDINALLY CONTINUOUS RIBBON OF PARTICLES OF UNIFORM SIZE AND SHAPE CONNECTED TOGETHER ALONG ADJACENT EDGE PORTIONS BY A WEB PORTION EXTENDING THE WIDTH OF SAID PATTERNED SURFACE, AND
2. A method of continuously forming uniform abrasive grains of desired size and shape from flowable thermoplastic vitreous or thermosetting ceramic material comprising: a. providing a pair of cooperating forming rollers rotatable about parallel longitudinal axes, b. providing patterned particle-forming surface portions on opposed surfaces of said forming rollers, c. supplying a flow of said material to the bite of said cooperating rollers, d. synchronizing said pair of cooperating rollers so that opposed patterned surface portions cooperate with one another, e. roll-forming between said cooperating rollers a longitudinally continuous ribbon of a plurality of adjacent particles connected together by means of a continuous connecting thin web portion extending across the width of the patterned surface portions and having opposed apexes which extend outwardly from opposite sides of the ribbon such that the plane of said web portion perpendicularly bisects an axis extending between a pair of opposed apexes, and f. flexing said ribbon between a pair of off-set rolls in various directions out of the plane of the ribbon to separate the newly formed abrasive particles therefrom along adjacent edge portions into individual particles of desired uniform size and shape for use as abrasive grains.
3. A method of continuously forming uniform abrasive grains of desired size and shape from flowable siliceous material comprising: a. providing a pair of cooperating forming rollers rotatable about parallel longitudinal axes, b. providing patterned particle-forming surface portions on opposed surfaces of said forming rollers, c. supplying a flow of siliceous material to the bite of said cooperating rollers, d. roll-forming between said cooperating rollers a longitudinally continuous ribbon of particles of uniform size and shape connected together along adjacent edge portions by interconnected web portions, e. metallizing said particles of siliceous material while in said ribbon form to form cermet abrasive grains, and f. flexing said ribbon of abrasive grains between a pair of off-set rolls in various directions out of the plane of the ribbon to separate the newly formed abrasive grains therefrom along adjacent edge portions into indivIdual abrasive particles of desired uniform size and shape.
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
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US253186A US3859407A (en) | 1972-05-15 | 1972-05-15 | Method of manufacturing particles of uniform size and shape |
FR7234480A FR2184579B1 (en) | 1972-05-15 | 1972-09-29 | |
DE2324111A DE2324111A1 (en) | 1972-05-15 | 1973-05-12 | PROCESS FOR PRODUCING PARTICLES OF THE SAME SHAPE AND SIZE |
JP48053476A JPS4941274A (en) | 1972-05-15 | 1973-05-14 | |
GB2303473A GB1416788A (en) | 1972-05-15 | 1973-05-15 | Forming particles having uniform size and shape |
US05/577,473 US4261706A (en) | 1972-05-15 | 1975-05-14 | Method of manufacturing connected particles of uniform size and shape with a backing |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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US253186A US3859407A (en) | 1972-05-15 | 1972-05-15 | Method of manufacturing particles of uniform size and shape |
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US05469449 Division | 1974-05-13 |
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US253186A Expired - Lifetime US3859407A (en) | 1972-05-15 | 1972-05-15 | Method of manufacturing particles of uniform size and shape |
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US (1) | US3859407A (en) |
JP (1) | JPS4941274A (en) |
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Also Published As
Publication number | Publication date |
---|---|
GB1416788A (en) | 1975-12-10 |
JPS4941274A (en) | 1974-04-18 |
FR2184579B1 (en) | 1976-08-20 |
DE2324111A1 (en) | 1973-12-06 |
FR2184579A1 (en) | 1973-12-28 |
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