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WO2004009269A2 - Amelioration d'une colle pour pastille - Google Patents

Amelioration d'une colle pour pastille Download PDF

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Publication number
WO2004009269A2
WO2004009269A2 PCT/US2003/023151 US0323151W WO2004009269A2 WO 2004009269 A2 WO2004009269 A2 WO 2004009269A2 US 0323151 W US0323151 W US 0323151W WO 2004009269 A2 WO2004009269 A2 WO 2004009269A2
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WO
WIPO (PCT)
Prior art keywords
filter
pellet
inoculating
weight
inoculant
Prior art date
Application number
PCT/US2003/023151
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English (en)
Other versions
WO2004009269A3 (fr
Inventor
Donald Craig
Karen Bingham
Leonard Aubrey
Original Assignee
Donald Craig
Karen Bingham
Leonard Aubrey
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Donald Craig, Karen Bingham, Leonard Aubrey filed Critical Donald Craig
Priority to AU2003252142A priority Critical patent/AU2003252142A1/en
Publication of WO2004009269A2 publication Critical patent/WO2004009269A2/fr
Publication of WO2004009269A3 publication Critical patent/WO2004009269A3/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D43/00—Mechanical cleaning, e.g. skimming of molten metals
    • B22D43/001—Retaining slag during pouring molten metal
    • B22D43/004—Retaining slag during pouring molten metal by using filtering means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D1/00—Treatment of fused masses in the ladle or the supply runners before casting
    • B22D1/007—Treatment of the fused masses in the supply runners
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
    • C21C1/00—Refining of pig-iron; Cast iron
    • C21C1/08—Manufacture of cast-iron

Definitions

  • the present invention is related to an improved inoculation filter and inoculation filter system for inoculating cast iron late in the casting process and to improvements in the adhesion between the inoculant pellet and the filter.
  • Cast iron is an extremely versatile engineered material comprising iron-carbon-silicon alloys that have been used in many commercial applications including the manufacture of mechanical parts.
  • the versatility of cast iron has led to the utilization of this material in many structural applications where the homogeneity and consistency of the iron will have a critical impact on the components performance.
  • the casting of clean homogenous iron, specifically grey or ductile is an essential step in the production of high quality engineered castings. Due to the importance of these cast items it is imperative that iron, specifically gray or ductile iron, be consistently cast with uniform morphology, with minimum included impurities and with properties that are reproducible.
  • Cast iron has an unusual metallurgical structure. Most metals form a single metallic crystalline structure during solidification. Cast iron, however, has a far more complex morphology during solidification. The crystalline phases that form during solidification of cast iron are dependent on the rate of solidification. Most engineered castings desire the formation of crystalline graphite within the iron matrix during solidification. If the cast iron solidifies too rapidly primary iron carbides can crystallize within the casting. Primary iron carbide is a hard brittle phase that makes the iron very difficult to machine and changes the physical and mechanical properties of the primary cast iron. Primary iron carbides are commonly referred to as "chill".
  • Carbon contained as iron carbides is generally considered to be detrimental in most iron castings whereas carbon present as graphite improves the physical and mechanical properties of cast iron.
  • Carbon can crystallize as either iron carbide or graphite during solidification. The formation of either phase is driven by the rate of solidification and the degree of nucleation contained within the liquid iron. The rate of solidification is constrained by the geometry of the casting, the rate of heat extraction of the mold material and the amount of superheat of the iron contained when the metal entered the mold. The degree of nucleation is constrained by the metallurgical history of the molten iron.
  • Carbon present as graphite is an advantageous form and persuading carbon to crystallize as graphite is an ongoing 'goal of standard foundry operations.
  • Graphite can be present in several morphological forms including spherical, as is the case with ductile iron, and flake-like, which is the case with gray iron.
  • Standard foundry metallurgical practice includes inoculation wherein the nucleation and growth of graphite is encouraged at the expense of iron carbide formation. Preferential nucleation greatly enhances the mechanical and physical properties of the finished casting. Inoculation is typically done by addition of an inoculating agent to either the pouring ladle, the metal stream or within the mold.
  • the inoculating agent is typically added to the pouring ladle by pouring the granulated inoculating agent into the ladle when the ladle is filled with liquid iron, whereas the inoculant is added to the metal stream by injecting or spraying a finely divided powder of the inoculating agent in the molten metal stream as the molten metal enters the mold. It is typically desirable to add the inoculating agent to the molten metal as late as possible to minimize fading. Insufficient or improper inoculation is constantly at the forefront of losses due to poor quality in a foundry operation.
  • the formed graphite may be spheroidal, if a spheroidal graphite cast iron called "SG " or "ductile” iron is required. Alternatively, a lamellar graphite cast iron is required for "LG” or “grey” iron. The essential prior condition to be met is to prevent the formation of primary iron carbide.
  • the liquid cast iron is subject before casting to an inoculation treatment, which will, as it cools, favour the appearance of graphite rather than that of primary iron carbide.
  • the inoculation treatment is therefore very important. It is in fact well known that the effectiveness of inoculation, whatever the inoculants used, reduces with time and, generally, has already reduced by 50% after a few minutes. To obtain maximum effectiveness, one skilled in the art generally practices progressive inoculation, applying to this end several additions of inoculants at different stages of the development of the cast iron. The final addition is made in the mold as the molds are fed or even in the feed conduits of the molds by placing in the path of the liquid cast iron inserts constituted by an inoculant material.
  • inserts are generally used associated with a filter; in this case they generally have a perfectly defined shape in order to be able to be fixed in the filter, most often in an adapted cavity.
  • inserts of defined shape are known as "pellets” or “slugs”.
  • filter inoculant package the unit constituted by the pellet and the filter.
  • pellets There are two types of pellets. “Molded” pellets are obtained by molding the molten inoculant. “Agglomerated” pellets are obtained from a pressed powder with generally very little binding agent, or even without binding agent.
  • Pellet inoculation wherein the molten metal is exposed to a pellet just prior to a filter, is known wherein a base material comprising minor amounts of calcium, aluminum, and rare earths are used.
  • a base material comprising minor amounts of calcium, aluminum, and rare earths are used.
  • the inoculation efficiency changes with time due to the kinetics associated with dissolution of the inoculating agent from the pellet.
  • various pour volumes and times are desired for manufacturing different parts with different sizes. If long pour times are utilized, the method of ladle inoculation is undesirable due to fading of the inoculant in the ladle. If short pour times are utilized, the time may by insufficient to allow for the onset of inoculation by pellet inoculation.
  • the properties which allow for effective inoculation in the metal stream are not well understood and typically a suitable working range is developed by experimentation at great cost and loss of material.
  • the Daussan patent FR 2,692,654 describes a filter inoculant package wherein the pellet is obtained by agglomeration of powder at 0.5 to 2 mm preferentially. The efficiency of this filter inoculant package is quite limited.
  • the Foseco Patent EP 0 234 825 describes a filter inoculant package wherein the inoculant is presented in the form of a powdery non-agglomerated powder enclosed in a plastic pouch. This unit is more complex to manufacture and employs non-agglomerated powder whose wettability with respect to the liquid cast iron is not always well controlled.
  • DE Patent Publication DE 43 18 309 Al incorporates an inoculating pellet into a depression of a filter.
  • the filter in a honeycomb, comprises pores of 1 to 8 mm.
  • the effectiveness of this type of filter inoculant package proves in use to be restricted by that of the pellet employed. This accomplishes the goal of inoculating late in the process but does not mitigate the primary issue associated with the process dependent inoculation efficiency described above.
  • the pellet/filter combination has been found to be of limited value to foundries since it does not provide any benefit, other than localizing the pellet.
  • 6,293,988 provides an inoculating agent which comprises oxysulphides.
  • the advantage provided is the elimination of ferrosilicon as a carrier medium.
  • the oxysulphide inoculating agent dissolves slowly and the rate of inoculation, particularly early in the pour, may be inconsistent and unpredictable.
  • a slowly dissolving pellet is subject to problems associated with inefficient inoculation early in the pour even though the problem of fade may be mitigated to some extent.
  • ferrosilicon carriers are known to dissolve very rapidly and therefore there use for ladle inoculation is widely accepted.
  • the rapid dissolution rate has caused ferrosilicon carrier based inoculants to be overlooked in the art due to the understanding that the rapid rate of dissolution would cause the pellet to be dissolved prior to the end of the pour and therefore the inoculant would not be effective throughout the entirity of the pour.
  • the rapid dissolution rate has made the ferrosilicon based inoculant difficult to control.
  • the filter inoculation system utilizes a friction fit inoculant in a partially bored filter element. While this product greatly improves the art of inoculation several problems exist which have been mitigated in the present invention.
  • the incorporation of a partial bore increases the manufacturing complexity thereby increasing cost. Furthermore, the additional manipulation increases spoilage. It would therefore be desirable to create a inoculant filter wherein the inoculant pellet is secured to the surface of the filter thereby obviating the need for a bore.
  • a particular feature of the present invention is reduction in the losses which occur during manufacturing and shipping.
  • Yet another particular feature of the present invention is the ability to minimize the necessity for a bore in the filter.
  • a method for securing an inoculating pellet to a filter comprising the steps of: applying a molten hot melt adhesive to the pellet; and contacting the filter with the pellet wherein the molten hot melt adhesive is between the pellet and the filter.
  • the method comprises the steps of forming a pellet by compressing a powdered inoculant into a cylinder. A ceramic filter is formed and a molten hot melt adhesive is placed between the filter pellet.
  • an inoculating filter comprising: an inoculating pellet, a ceramic filter and a hot melt adhesive there between.
  • a particularly preferred embodiment is provided in a method for inoculating molten iron.
  • the method comprises passing the molten iron through a filter assembly.
  • the filter assembly comprises a filter element, an inoculation pellet and a hot melt adhesive between the filter element and the pellet.
  • Fig. 1 is a cross-sectional view of a test mold.
  • Fig. 2 is a top view of an inoculant pellet attached to a filter in the bore.
  • FIG. 3 is a perspective view of an inoculant pellet attached on top of the filter.
  • the present invention relates to an inoculation system comprising an inoculation pellet in functional contact with a filter element and to a method for use which greatly increases the consistency with which molten metal, particularly iron, can be inoculated.
  • molten metal particularly iron
  • the art of inoculation with a pellet has previously met with limited success.
  • Non-ferrosilicon based pellets, such as those described in U.S. Pat. No. 6,293,988 dissolve slowly and the resulting cast iron still comprises chill levels which are consistent with inappropriate inoculation.
  • the art lacks a teaching which provides a ferrosilicon based inoculant pellet which can be utilized over a broad range of flow rates, or approach velocities, with adequate inoculation and minimal fading and which can be manufactured and transported with minimal loss. Through diligent research such teaching is provided herein.
  • Fig. 1 illustrates a test mold for preparing cast of molten iron for determination of effectiveness.
  • the test mold generally represented at 1, comprises a mold cavity, 2, into which the molten metal will flow and cool. Spacers, 3, are placed between the mold cavity, 2, and an upper pouring cup 4.
  • the filter, 6, and pellet, 7, are held into a funnel, 5. Molten metal is poured into the funnel, 5, whereby it passes through the filter and dissolves the pellet. The dissolution of the pellet imparts inoculants into the molten metal.
  • the molten metal flow through the channel, 8, in the spacers, 3, and into the mold cavity, 2.
  • a pellet and filter are illustrated in top view in Fig. 2 and perspective view in Fig. 3.
  • the pellet, 7, is secured to the filter by the adhesive, 9.
  • 0.2 to 2 mm granulated particles are used during ladle treatment, and 0.2 to 0.7 mm granulated particles are used for stream inoculation when casting.
  • the applicant has in fact noted an unexpected phenomenon in the testing shop.
  • the number of graphite nuclei generated in the liquid cast iron increases with the number of inoculant particles added to the inoculant mass unit. Therefore, if two ladles of cast iron are treated in identical conditions with a same inoculant in two different particle size distributions, the cast iron treated with the finest product will contain more graphite nuclei that that treated with the coarser product. These nuclei will also be smaller in size.
  • a powder of this type agglomerates easily which makes it possible to operate with lower proportions of binding agent.
  • sodium silicate which is a well known binding agent
  • doses of 0.3 cm 3 for 100 g of powder to 3 cm 3 for 100 g of powder are sufficient according to the pressures employed which may vary from 50 to 500 MPa since the mechanical performance of the pellets is easily acquired.
  • the pressure and binding agent percentage parameters may be used to control the dissolution speed of the pellet and not its mechanical performance.
  • the filter associated with the pellet is a ceramic filter comprising continuous or semi-continuous voids or passageways which the metal passes and in which any included particles larger than 10 ⁇ and preferably 3 ⁇ become lodged.
  • the effective component of the present invention comprises a ferrosilicon carrier and at least one active element.
  • the ferrosilicon carrier is a low- active element which dissolves in molten iron without significantly forming seed nuclei.
  • the active element is an element, or combination of elements, which dissolve in molten iron and react with elements in the molten iron to form seed nuclei upon which graphite preferentially crystallizes.
  • the effective component of the inoculant pellet preferably comprises
  • ferrosilicon comprising non-reactive impurities.
  • Ferrosilicon is available commercially from a variety of sources. Ferrosilicon is typically provided as 75% ferrosilicon which indicates, by nomenclature in the art, that the material comprises approximately 75%, by weight, silicon and 25%, by weight, iron. Ferrosilicon is widely available as 50% ferrosilicon which indicates that the material comprises approximately 50%, by weight, silicon and 50%o, by weight, iron.
  • the binder includes all non-inoculating elements. It is most preferred that the carrier comprise at least about 30%, by weight ferrosilicon.
  • the active elements of the present invention include at least one rare earth or at least one inoculating agent chosen from the group consisting of cerium, strontium, zirconium, "calcium, manganese, barium, bismuth, magnesium, titanium, aluminum, lanthanum and sulfur.
  • Particularly preferred inoculating agents include at least one element chosen from the group consisting of strontium, aluminum, lathanum, zirconium, calcium and manganese.
  • the inoculant preferably comprises about 0.1-60%), by weight inoculating agent.
  • the inoculant comprises about 0.1-40%, by weight, active inoculating agent. Most preferably, the inoculant comprises about 0.1- 20%, by weight, active inoculating agent.
  • Approach velocity is a practical measure, well known in the industry, to indicate the volume of metal flowing to, and through, a filter. As would be apparent to one of ordinary skill in the art the approach velocity is determined at a fixed cross- sectional flow area. For the purposes of the present invention all approach velocities are calculated at a cross-sectional area of 30.25 cm 2 unless otherwise stated. It would be readily apparent to one of ordinary skill in the art that different cross-sectional areas would generate different approach velocities, however, the approach velocity could be easily compared to those cited herein by simple conversion as known in the art.
  • the dissolution rate of the inoculant is defined as the amount of inoculating agent consumed as a function of time.
  • the analysis of certain inoculants is difficult therefore the dissolution rate is based on the analysis of a determinant element, either an inoculant or marker.
  • the weight ratio of the determinant element to other inoculating agents is assumed to be the same in the cast iron as the weight ratio in the original pellet.
  • zirconium is used as an inoculating determinate element. Therefore, the total inoculant in the cast iron is determined as the amount of zirconium plus other inoculants in the iron.
  • an inoculant has 1 part zirconium, by weight, to 1 part manganese, by weight, and the amount of zirconium in the iron is 20 ppm then the amount of manganese will also be 20 ppm for a total inoculant of 40 ppm.
  • the grams of zirconium plus manganese, which is present in an amount of 40 ppm, divided by the pour time is the inoculant dissolution rate.
  • An inoculant dissolution rate of at least approximately 1 mg/sec. is necessary to have sufficient inoculation for approach velocities of 1-60 cm/sec. Below 1 mg/sec. an insufficient inoculation rate is observed, particularly early in the pour, to insure minimum or no chill and to substantially eliminate the formation of iron carbide.
  • the approach velocity must be lowered to a level which is impractical with an inoculant dissolution rate below approximately 1 mg/sec. More preferably, the inoculant dissolution rate is no less than 10 mg/sec. More preferably, the inoculant dissolution rate is no less than 20 mg/sec. An inoculant dissolution rate of no more than approximately 320 mg/sec.
  • the inoculant dissolution rate is no more than approximately 250 mg/sec. Most preferably, the inoculant dissolution rate is no more than approximately 200 mg/sec.
  • ferrosilicon based inoculants dissolve at a rate which exceeds 320 mg/sec. While imminently suitable for use in ladle inoculation these have been found to be unsuitable for use in a pellet at the point of filtration. Prior to the present invention the rate of dissolution for ferrosilicon based inoculants has not been explored due to the understanding in the art that the rate was to fast to be applied in this manner.
  • the present invention illustrates that a ferrosilicon based inoculant can be prepared which, when prepared to a narrow range of dissolution rate, can be utilized as an inoculant pellet and the resulting cast iron has a low level of chill.
  • a dissolution rate of approximately 1 to approximately 320 mg/sec. allows for an inventive pellet to by used at approach velocities of 1-60 cm/sec. without fade or under inoculation in any portion of the pour. This is currently not available in the art without utilizing very large pellets which are only partially used or approach velocities which are undesirable. More preferably, the dissolution rate is approximately 1 to approximately 320 mg/sec.
  • the dissolution rate of the pellet is determined at an approach velocity of 15 cm/sec. measured at a cross-sectional area of 30.25 cm 2 .
  • the pellet preferably has a dissolution rate of at least approximately 2 mg/sec. to no more than approximately 300 mg/sec. More preferably, measured at an approach velocity of 15 cm/sec. the pellet has a preferred dissolution rate of at least approximately 2 mg/sec. to no more than approximately 200 mg/sec.
  • the filtration rate of the filter can be adjusted between 0.01 kg/(s cm 2 ) and 0.5 kg/(scm 2 ). More preferably between 0.04 kg/(s cm 2 ) and 0.24 kg/(s'cm ) according to the application.
  • the filter inoculant package is sized with a ratio (pellet mass in g/filter surface in cm ) between 0.75 and 1.5.
  • a filter inoculant package made of a 25 g pellet and a 30 cm 2 filter would be a convenient sizing.
  • the dissolution rate of the pellet is controlled by composition and packing density and particle size distribution. As the packing density increases the dissolution rate decreases.
  • a ferrosilicon binder compressed to achieve a density of approximately 2.3 g/cc to approximately 2.6 g/cc is suitable to obtain the dissolution range required for the invention.
  • Such a result can be obtained in adjusting the density of a pellet which can be obtained between 60% and 80%) of the true density of the inoculant alloy the pellet is made of, depending on the pressure used for agglomerating which can vary from 50 to 500 MPa.
  • Filter inoculant packages according to the invention may be sized for the treatment of molten iron flow rates between 1 and 25 kg/s.
  • Ceramic filter elements are porous members comprising continuous or semi-continuous voids or passageways through which the metal passes and in which any included particles become lodged.
  • the porous ceramic filter elements are preferably prepared by the manner described in U.S. Patent No. 4,056,586, which is incorporated herein by reference. Further elaboration on methods for manufacturing ceramic filter elements is provided in U.S. Patent Nos. 5,673,902 and 5,456,833, both of which are included herein by reference.
  • Typical hot melt adhesives are made with a base polymer which is a polymeric thermoplastic material which is solid at about 70°F.
  • the base polymer is typically compounded 'with one or more tackifiers and preferably one or more waxes.
  • the low-density hot melt adhesives are typically made by adding a low-density filler to a hot melt adhesive.
  • the preferred base polymers are the following, or mixtures thereof: polyethylene, polypropylene, polybutene, ethylene-vinyl acetate (EVA), ethylene ethyl acrylate, ethylene-acrylic acid, ethylene propylene copolymer, ethylene propylene butene terpolymer and styrene block copolymer.
  • EVA ethylene-vinyl acetate
  • ethylene ethyl acrylate ethylene-acrylic acid
  • ethylene propylene copolymer ethylene propylene butene terpolymer
  • styrene block copolymer ethylene-vinyl acetate
  • EVA ethylene-vinyl acetate
  • ethylene ethyl acrylate ethylene-acrylic acid
  • propylene copolymer ethylene propylene butene ter
  • tackifiers should be compatible with the base polymer, should not separate upon standing in liquid or molten form, and are preferably highly oxidatively stable.
  • naturally-occuring resins which may be used are polyterpenes, rosins, rosin esters and derivatives thereof.
  • Hydrocarbon resins particularly those with 5 and 9 carbons, terpenes, terpene/phenolics, polymerized a- and b- pinenes, rosin-modified phenolic resins, polymerized rosin, rosin derivatives, such as hydrogenated and dimerized rosins, and tall oil rosins may be used as tackifiers.
  • tackifying resins may also be employed, examples of which include aliphatic and aromatic hydrocarbon resins. Examples of other resins which may be used included modified terpenes, coumarone-indenes, polyesters, alkyl phenols, and stryrene oligomers. Mixtures of tackifiers may also be used. The tackifier is present in an effective amount, to lower the melt viscosity of the composition and improve its ability to wet the substrate, thereby improving adhesion to the substrate. One percent tackifer, by weight, is particularly suitable. Hot melt adhesive compositions may contain at least 1 weight percent of one or more wax, which are generally low-melting hydrocarbon materials.
  • Waxes may be included to raise or lower the softening point, to improve set times of the adhesive composition, to alter its viscosity, to improve handling characteristics and/or to increase the hardness of the bond provided.
  • Suitable waxes include low molecular weight polyethylene, microcrystalline wax, Fischer-Tropsch wax, synthetic hydrocarbon wax, paraffin wax, and mixtures of these waxes.
  • Preferred hot melt adhesives include 10-99.7%), by weight, more preferably 20-80%>, by weight, more preferably 30-60%>, by weight base polymer; 0- 85%, by weight, more preferably 10-50%, by weight, tackifier; 0-50%, by weight, more preferably 0-20%, by weight, more preferably 5-15%, by weight, wax and 0-10%), by weight, more preferably 0.5-5%, by weight, and more preferably 1-3%, by weight low density filler.
  • the weight percent of low-density filler may vary beyond these ranges depending on the density thereof.
  • Hot melt adhesives, tackifiers and waxes are well known in the art as exemplified in U.S. Pat. Nos. 5,672,677; 5,454,909; 5,026,752; 4,882,414; 4,853,460 and 4,283,317 all of which are incorporated by reference.
  • Examples 1 to 5 are related to ductile cast irons.
  • Example 6 is related to grey cast iron EXAMPLE 1
  • a series of 30.25 cm 2 square silicon carbide ceramic filters were prepared using standard techniques.
  • a charge of cast iron was melted in the induction furnace and treated by the Tundish Cover process by means of an alloy of the FeSiMg type with 5%> Mg, 2% Ca, and 2% total rare earths (TRE) at the dose of 20 kg for 1600 kg of cast iron.
  • This cast iron was used to cast parts with a unit mass of about 1 kg, placed in clusters in a 20 part mold fed by an inflow conduit in which was placed a molded pellet of batch "B". The number of graphite nodules observed by metallography on the cross-section of the parts was 184/mm 2 .
  • Example No. 2 was reproduced in an identical way with the sole difference that the molded slug coming from batch "B" was replaced with an agglomerated pellet according to the prior art obtained by pressing a powder 0 to 2 mm obtained by natural crushing of molded pellets taken from the same batch "B” as the pellet used in the previous example.
  • the particle size distribution of this powder was: passing to 2 mm: 100%; passing to 0.4 mm: 42%; passing to 0.2 mm: 20%; passing to 50 ⁇ : 10%, i.e. a particle size distribution quite close to that recommended in EP 0 234 825.
  • the number of graphite nodules observed by metallography on the cross-section of the parts was 168/mm 2 .
  • Example No. 3 was reproduced in an identical way with the sole difference that the molded slug came from batch "A".
  • the number of graphite nodules observed by metallography on the cross-section of the pellets was 170/mm 2 .
  • Example No. 3 was repeated with the following conditions. A 25 kg batch of molded slugs from batch "B" was crushed to 0 to 1 mm. The fractions 0.63 to
  • Example No. 5 was repeated with the following conditions.
  • a charge of 1600 kg of cast iron was melted in an induction furnace.
  • the eutectic temperature was 1136°C.
  • the cast iron was used to cast parts with a unit mass of about 1 kg, placed in clusters in a 20 part mold fed by an inflow conduit in which was placed a molded pellet supported by a 30.25 cm 2 filter constituted by a refractory foam identical to the ones used in the other examples.
  • the molded slug was from batch "C".
  • EXAMPLE 7 [00063] A series of 30.25 cm 2 square silicon carbide ceramic filters were prepared using standard techniques. An organic foam was coated with a ceramic slurry such that all voids were filled. The organic foam was then compressed to expel excess slurry there from while leaving the organic foam coated with slurry. The coated organic foam slurry was then dried and fired. A circular void, approximately 25.4 mm in diameter, was cut partially into a surface of the filter for fitting of the pellet.
  • a series of cylindrical pellets approximately 20.5 mm in thickness and approximately 25.4 mm in diameter were prepared creating an alloy of active ingredients with silicon and iron.
  • the alloy was melted, crushed, pulverized, sized and mixed with sodium silicate to form a pellet.
  • the powder was placed in a mold and compressed to a level sufficient to obtain the density required of approximately 2.3 to 2.6 g/cc. The pellet was then inserted into the circular void of the ceramic filter.
  • a test mold comprising 5 chambers of equal size wherein each chamber is filled sequentially in a single pour was used to determine the dissolution rate of the pellet/filter combination throughout the pour.
  • the pellet/filter combination was inserted into the test mold prior to the chambers and 29.51 Kg of molten iron was poured into the mold over different periods of time. Temperatures during the pour were determined to range from 1335-1470°C with no significant difference noted within this range of temperature.
  • a ferrosilicon pellet was prepared as in the inventive example except the particle size and packing as commonly employed in ferrosilicon based inoculants.
  • the dissolution rate was estimated by pellet loss analysis and inoculant element percentage. The results are provided in Table 2.
  • a round inoculation disk with a diameter of 26.4 mm and a thickness of approximately 17 mm was inserted into a SELEE® silicon carbide filter.
  • the inoculation disk comprised 15-49%, by weight, silicon; 7-22%, by weight, calcium; 2.5- 10%, by weight, sulfur; 2.5-7.5%, by weight, magnesium and 0.5-5%, by weight, aluminum.
  • Samples of 20kg-29kg Gray iron were poured through the filter at an approach velocity of approximately 12-18 cm/sec. After the pour was complete the remaining pellet was analyzed by SEM/EDS. A similar analysis was not possible with the inventive examples since the pellet was no longer distinguishable. The analysis suggested the formation of complex dross formations including silicates and sulfides of calcium magnesium aluminum compounds.
  • test molds were poured they were allowed to cool to room temperature.
  • the filter was then examined to determine if any residual inoculant was contained within the filter body.
  • the dissolution of the inoculant tablet was ranlced on a scale of 1 to 10. A rank of 1 represents no visible dissolution whereas a rank of 10 represents complete dissolution.
  • the inoculant filter for this testing utilized a 15 g tablet comprising a binder and method of assembly as described in Table 3.
  • the dissolution of the inoculant tablet was ranlced for each tablet tested. Table 3 describes the set up and factors that were varied during the experimentation and the results. All experiments were repeated once to confirm test results. The results from the first heat and second heat were identical.
  • Table 3 clearly shows that a change in the binder system decreases the dissolution rate of the inoculant tablet. This is undesirable.
  • the tablets with PVA binder were more durable.
  • Table 3 also illustrates that the type of adhesive has an impact on the dissolution of the tablet.
  • Sodium silicate is used as the binder and does not negatively impact the dissolution of the tablet.
  • sodium silicate was used as the adhesive it had a negative effect on the dissolution behavior of the tablet.
  • Coating the tablet with sodium silicate completely retarded the dissolution behavior of the tablet. This is surprising due to the observation that the sodium silicate is a preferred binder.
  • the adhesive, and the method of application have a direct impact on the dissolution behavior of the inoculant tablet. This finding is unexpected.
  • Table 4 describes additional test factors.
  • the test utilized a 15 gram pellet comprising a sodium silicate binder. All pellets were substantially identical.
  • Heat 1 was done with a charge mix of gray iron returns (285 lb.) and steel punchings (7 lb.) for a total charge of 292 Tbs.
  • the chemical composition was determined to be CE, 3.89 %; C, 3.33%; and Si, 1.68%, by weight.
  • the tapping temperature was 2652°F; the temperature in the ladle was 2604°F and the temperature at the end of the pour was 2502°F.
  • the whole pouring cycle of 6 molds was approximately 3 min.
  • Heat 2 was done with a charge mix of gray iron returns (285 lbs.) and steel punching (10 lbs.) for a total charge mix of 295 lbs.
  • the chemical composition was CE 4.04%; C, 3.39% and Si, 1.92% .
  • the tapping temperature was 2654°F, the temperature in the ladle was 2613°F and the temperature at the end of the pouring was
  • Heat 3 was done with a charge mix of 250 lbs. of gray iron returns.
  • Hot Melt Adhesive A is a hot melt EVA-based, medium setting, adhesive available as Hysol® Product 1942 from Loctite of Rock Hill, Ct.
  • Hot Melt Adhesive A has a softening point of 198 °F (ASTM E28-67); a viscosity @350°F of 5000 cP (ASTM D 3236); a open time of 30 seconds; a heat resistance of 142 °F (ASTM D 4498), a specific gravity of 0.96 @ 77 °F (ASTM D 792); a tensile strength of 250 psi (ASTM D 638); an elongation of 500% (ASTM D 1876), a Tg of 7 °F (ASTM E 1640) and a "T" peel aluminum of 44 pli (ASTM D 1876).
  • Hot Melt Adhesive B is a hot melt EVA-based, medium setting, adhesive available as Hysol® Product 232 from Loctite of Rock Hill, Ct.
  • Hot Melt Adhesive A has a softening point of 188 °F (ASTM E28-67); a viscosity @350°F of 11000 cP (ASTM D 3236); a open time of 15 seconds; a heat resistance of 153 °F (ASTM D 4498), a specific gravity of 0.96 @ 77 °F (ASTM D 792); a tensile strength of 150 psi (ASTM D 638); a Tg of -22 °F (ASTM E 1640) and an elongation of 1500% (ASTM D 638).
  • Table 5 illustrates that the type of adhesive and the method employed to apply the adhesive has an impact on both dissolution behavior of the tablet and the durability of the inoculant filter product. It is critical that the type of adhesive and the method used to apply the adhesive keeps the inoculant tablet firmly attached to the filter body. It was clearly evident that placing the adhesive at the bottom of the hole drilled in the filter body is ineffective in holding the tablet in place during shipment. Placing a bead of adhesive on the circumference of the pellet in a manner that allows good contact of the adhesive on both sidewalls of the filter and the tablet is an effective method of applying the adhesive. The finding that the method of applying the adhesive to the filter and or the inoculant filter was not expected to have such a dramatic effect on the transportation of the product.
  • Table 5 illustrates that the selection of adhesive does impact the dissolution behavior of the inoculant tablet.
  • the PVA adhesive has a negative impact the dissolution of the tablet.
  • the hot melt adhesives worked better than the PVA adhesive or the sodium silicate adhesive.
  • Hot Melt Adhesive B is most preferred.
  • the inoculant tablet dissolved almost completely in the test mold. This finding was completely unexpected and the fact that the type of adhesive would have such a dramatic effect on the dissolution behavior is not yet understood.
  • the Hot Melt Adhesive B has been tested and found to work effectively in both the shipment of the inoculant filters and in the dissolution of the tablets in test castings.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Refinement Of Pig-Iron, Manufacture Of Cast Iron, And Steel Manufacture Other Than In Revolving Furnaces (AREA)

Abstract

L'invention concerne un procédé de fixation d'une pastille d'inoculation à un filtre. Ce procédé consiste à appliquer une colle thermofusible (9) fondue sur une pastille (7) et à mettre en contact le filtre (6) avec la pastille, la colle thermofusible fondue étant intercalée entre la pastille et le filtre.
PCT/US2003/023151 2002-07-24 2003-07-24 Amelioration d'une colle pour pastille WO2004009269A2 (fr)

Priority Applications (1)

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AU2003252142A AU2003252142A1 (en) 2002-07-24 2003-07-24 Method for securing an inoculating pellet to a filter and inoculation filter thus obtained

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US39826802P 2002-07-24 2002-07-24
US60/398,268 2002-07-24

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Cited By (23)

* Cited by examiner, † Cited by third party
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US7175638B2 (en) 2003-04-16 2007-02-13 Satiety, Inc. Method and devices for modifying the function of a body organ
US7211094B2 (en) 2002-11-05 2007-05-01 Satiety, Inc. Magnetic anchoring devices
US7214233B2 (en) 2002-08-30 2007-05-08 Satiety, Inc. Methods and devices for maintaining a space occupying device in a relatively fixed location within a stomach
US7220237B2 (en) 2002-10-23 2007-05-22 Satiety, Inc. Method and device for use in endoscopic organ procedures
US7229428B2 (en) 2002-10-23 2007-06-12 Satiety, Inc. Method and device for use in endoscopic organ procedures
US7288099B2 (en) 2001-05-30 2007-10-30 Satiety, Inc. Obesity treatment tools and methods
US7306614B2 (en) 2001-05-30 2007-12-11 Satiety, Inc. Overtube apparatus for insertion into a body
US7534841B2 (en) 2004-10-21 2009-05-19 Basell Polyolefine Gmbh 1-butene polymer and process for the preparation thereof
US7708684B2 (en) 2004-02-27 2010-05-04 Satiety, Inc. Methods and devices for reducing hollow organ volume
US7753870B2 (en) 2004-03-26 2010-07-13 Satiety, Inc. Systems and methods for treating obesity
US7753928B2 (en) 2000-11-03 2010-07-13 Satiety, Inc. Method and device for use in minimally invasive placement of intragastric devices
US7757924B2 (en) 2004-02-05 2010-07-20 Satiety, Inc. Single fold system for tissue approximation and fixation
US7914543B2 (en) 2003-10-14 2011-03-29 Satiety, Inc. Single fold device for tissue fixation
US8007505B2 (en) 2003-10-14 2011-08-30 Ethicon Eado-Surgery, Inc. System for tissue approximation and fixation
US8062207B2 (en) 2002-08-07 2011-11-22 Ethicon Endo-Surgery, Inc. Intra-gastric fastening devices
US8092378B2 (en) 2004-11-17 2012-01-10 Ethicon Endo-Surgery, Inc. Remote tissue retraction device
US8092482B2 (en) 2002-08-30 2012-01-10 Ethicon Endo-Surgery, Inc. Stented anchoring of gastric space-occupying devices
US8252009B2 (en) 2004-03-09 2012-08-28 Ethicon Endo-Surgery, Inc. Devices and methods for placement of partitions within a hollow body organ
US8257365B2 (en) 2004-02-13 2012-09-04 Ethicon Endo-Surgery, Inc. Methods and devices for reducing hollow organ volume
US8449560B2 (en) 2004-03-09 2013-05-28 Satiety, Inc. Devices and methods for placement of partitions within a hollow body organ
US8628547B2 (en) 2004-03-09 2014-01-14 Ethicon Endo-Surgery, Inc. Devices and methods for placement of partitions within a hollow body organ
CN103949591A (zh) * 2014-03-31 2014-07-30 日月重工股份有限公司 用于铸造化学标准样毛坯的浇注系统
US9028511B2 (en) 2004-03-09 2015-05-12 Ethicon Endo-Surgery, Inc. Devices and methods for placement of partitions within a hollow body organ

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EP0410603A1 (fr) * 1989-07-26 1991-01-30 Foseco International Limited Coulée de la fonte liquide et filtres utilisés
FR2691654A1 (fr) * 1992-05-29 1993-12-03 Daussan & Co Procédé pour traiter du métal en fusion dans une opération de coulée avec interposition d'un filtre, et filtre pour la mise en Óoeuvre de ce procédé.
DE4318309A1 (de) * 1993-06-02 1994-12-08 Sueddeutsche Kalkstickstoff Keramikfilter für Metallschmelzen mit integriertem Behandlungsmittel
US6293988B1 (en) * 1998-08-04 2001-09-25 Rodney Louis Naro Inoculant and inoculant method for gray and ductile cast irons

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Publication number Priority date Publication date Assignee Title
DE1608051A1 (de) * 1968-02-27 1970-10-22 Stettner & Co Siebkern fuer die Formimpfung von Stahl- und Gusseisenschmelzen und Verfahren zu seiner Herstellung
EP0410603A1 (fr) * 1989-07-26 1991-01-30 Foseco International Limited Coulée de la fonte liquide et filtres utilisés
FR2691654A1 (fr) * 1992-05-29 1993-12-03 Daussan & Co Procédé pour traiter du métal en fusion dans une opération de coulée avec interposition d'un filtre, et filtre pour la mise en Óoeuvre de ce procédé.
DE4318309A1 (de) * 1993-06-02 1994-12-08 Sueddeutsche Kalkstickstoff Keramikfilter für Metallschmelzen mit integriertem Behandlungsmittel
US6293988B1 (en) * 1998-08-04 2001-09-25 Rodney Louis Naro Inoculant and inoculant method for gray and ductile cast irons

Cited By (56)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7753928B2 (en) 2000-11-03 2010-07-13 Satiety, Inc. Method and device for use in minimally invasive placement of intragastric devices
US8137366B2 (en) 2001-05-30 2012-03-20 Ethicon Endo-Surgery, Inc. Obesity treatment tools and methods
US8123765B2 (en) 2001-05-30 2012-02-28 Ethicon Endo-Surgery, Inc. Obesity treatment tools and methods
US8613749B2 (en) 2001-05-30 2013-12-24 Ethicon Endo-Surgery, Inc. Obesity treatment tools and methods
US8419755B2 (en) 2001-05-30 2013-04-16 Ethicon Endo-Surgery, Inc. Obesity treatment tools and methods
US7288099B2 (en) 2001-05-30 2007-10-30 Satiety, Inc. Obesity treatment tools and methods
US7288101B2 (en) 2001-05-30 2007-10-30 Satiety, Inc. Obesity treatment tools and methods
US7306614B2 (en) 2001-05-30 2007-12-11 Satiety, Inc. Overtube apparatus for insertion into a body
US7503922B2 (en) 2001-05-30 2009-03-17 Satiety, Inc. Obesity treatment tools and methods
US7510559B2 (en) 2001-05-30 2009-03-31 Satiety, Inc. Obesity treatment tools and methods
US8794243B2 (en) 2001-05-30 2014-08-05 Ethicon Endo-Surgery, Inc. Obesity treatment tools and methods
US8080022B2 (en) 2001-05-30 2011-12-20 Ethicon Endo-Surgery, Inc. Obesity treatment tools and methods
US8137367B2 (en) 2001-05-30 2012-03-20 Ethicon Endo-Surgery, Inc. Obesity treatment tools and methods
US8075577B2 (en) 2001-05-30 2011-12-13 Ethicon Endo-Surgery, Inc. Obesity treatment tools and methods
US8080025B2 (en) 2001-05-30 2011-12-20 Ethicon Endo-Surgery, Inc. Obesity treatment tools and methods
US7909838B2 (en) 2001-05-30 2011-03-22 Satiety, Inc. Obesity treatment tools and methods
US7862574B2 (en) 2001-05-30 2011-01-04 Satiety, Inc. Obesity treatment tools and methods
US8062207B2 (en) 2002-08-07 2011-11-22 Ethicon Endo-Surgery, Inc. Intra-gastric fastening devices
US8083756B2 (en) 2002-08-30 2011-12-27 Ethicon Endo-Surgery, Inc. Methods and devices for maintaining a space occupying device in a relatively fixed location within a stomach
US8083757B2 (en) 2002-08-30 2011-12-27 Ethicon Endo-Surgery, Inc. Methods and devices for maintaining a space occupying device in a relatively fixed location within a stomach
US7947055B2 (en) 2002-08-30 2011-05-24 Ethicon Endo-Surgery, Inc. Methods and devices for maintaining a space occupying device in a relatively fixed location within a stomach
US8092482B2 (en) 2002-08-30 2012-01-10 Ethicon Endo-Surgery, Inc. Stented anchoring of gastric space-occupying devices
US7214233B2 (en) 2002-08-30 2007-05-08 Satiety, Inc. Methods and devices for maintaining a space occupying device in a relatively fixed location within a stomach
US7789848B2 (en) 2002-10-23 2010-09-07 Satiety, Inc. Method and device for use in endoscopic organ procedures
US8147441B2 (en) 2002-10-23 2012-04-03 Ethicon Endo-Surgery, Inc. Method and device for use in endoscopic organ procedures
US8801650B2 (en) 2002-10-23 2014-08-12 Ethicon Endo-Surgery, Inc. Method and device for use in endoscopic organ procedures
US7220237B2 (en) 2002-10-23 2007-05-22 Satiety, Inc. Method and device for use in endoscopic organ procedures
US7229428B2 (en) 2002-10-23 2007-06-12 Satiety, Inc. Method and device for use in endoscopic organ procedures
US7211094B2 (en) 2002-11-05 2007-05-01 Satiety, Inc. Magnetic anchoring devices
US8231641B2 (en) 2003-04-16 2012-07-31 Ethicon Endo-Surgery, Inc. Method and devices for modifying the function of a body organ
US7175638B2 (en) 2003-04-16 2007-02-13 Satiety, Inc. Method and devices for modifying the function of a body organ
US9186268B2 (en) 2003-10-14 2015-11-17 Ethicon Endo-Surgery, Inc. Single fold device for tissue fixation
US8007505B2 (en) 2003-10-14 2011-08-30 Ethicon Eado-Surgery, Inc. System for tissue approximation and fixation
US8357174B2 (en) 2003-10-14 2013-01-22 Roth Alex T Single fold device for tissue fixation
US7914543B2 (en) 2003-10-14 2011-03-29 Satiety, Inc. Single fold device for tissue fixation
US7757924B2 (en) 2004-02-05 2010-07-20 Satiety, Inc. Single fold system for tissue approximation and fixation
US8590761B2 (en) 2004-02-05 2013-11-26 Ethicon Endo-Surgery, Inc. Single fold system for tissue approximation and fixation
US8828025B2 (en) 2004-02-13 2014-09-09 Ethicon Endo-Surgery, Inc. Methods and devices for reducing hollow organ volume
US8257365B2 (en) 2004-02-13 2012-09-04 Ethicon Endo-Surgery, Inc. Methods and devices for reducing hollow organ volume
US7708684B2 (en) 2004-02-27 2010-05-04 Satiety, Inc. Methods and devices for reducing hollow organ volume
US8057384B2 (en) 2004-02-27 2011-11-15 Ethicon Endo-Surgery, Inc. Methods and devices for reducing hollow organ volume
US8449560B2 (en) 2004-03-09 2013-05-28 Satiety, Inc. Devices and methods for placement of partitions within a hollow body organ
US8252009B2 (en) 2004-03-09 2012-08-28 Ethicon Endo-Surgery, Inc. Devices and methods for placement of partitions within a hollow body organ
US9028511B2 (en) 2004-03-09 2015-05-12 Ethicon Endo-Surgery, Inc. Devices and methods for placement of partitions within a hollow body organ
US8628547B2 (en) 2004-03-09 2014-01-14 Ethicon Endo-Surgery, Inc. Devices and methods for placement of partitions within a hollow body organ
US7753870B2 (en) 2004-03-26 2010-07-13 Satiety, Inc. Systems and methods for treating obesity
US7534841B2 (en) 2004-10-21 2009-05-19 Basell Polyolefine Gmbh 1-butene polymer and process for the preparation thereof
US8403838B2 (en) 2004-11-17 2013-03-26 Ethicon Endo-Surgery, Inc. Remote tissue retraction device
US8784306B2 (en) 2004-11-17 2014-07-22 Ethicon Endo-Surgery, Inc. Remote tissue retraction device
US8454503B2 (en) 2004-11-17 2013-06-04 Ethicon Endo-Surgery, Inc. Remote tissue retraction device
US8795166B2 (en) 2004-11-17 2014-08-05 Ethicon Endo-Surgery, Inc. Remote tissue retraction device
US8092378B2 (en) 2004-11-17 2012-01-10 Ethicon Endo-Surgery, Inc. Remote tissue retraction device
US8939902B2 (en) 2004-11-17 2015-01-27 Ethicon Endo-Surgery, Inc. Remote tissue retraction device
US8403839B2 (en) 2004-11-17 2013-03-26 Ethicon Endo-Surgery, Inc. Remote tissue retraction device
CN103949591A (zh) * 2014-03-31 2014-07-30 日月重工股份有限公司 用于铸造化学标准样毛坯的浇注系统
CN103949591B (zh) * 2014-03-31 2015-12-09 日月重工股份有限公司 用于铸造化学标准样毛坯的浇注系统

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AU2003252142A8 (en) 2004-02-09
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