FR2666819A1 - METHOD AND DEVICE FOR MANUFACTURING A COMPOSITE MATERIAL FROM A BASE METAL. - Google Patents

Abstract

The device comprises a crucible (10) housing a molten base metal, means (2) for producing a plasma for receiving a stream of inert gas and particles of an entrained charge and ionizing the gas and heating the particles, means (2) for injecting the gas and particles into the crucible so that they penetrate the molten metal in the crucible; means (4) for continuously stirring the molten metal in the crucible; a mold (6) receiving the molten metal containing the filler particles, and means (7) for continuously stirring the molten metal in the mold (6). Application in particular to the manufacture of composite materials in the field of aeronautics and the automotive industry.

Description

i The present invention relates to the field of metallurgy and, so

  more specifically, a process for producing a molded base metal material in which are distributed very fine particles, which may be particles of ceramics, metals, alloys, intermetallic materials, carbide, nitride, boride and substances useful for improving the properties of

base metal.

  The development of aeronautics and

  shipbuilding, automotive industry and some

  many other industries require new materials

  rials with machinability and

improved service.

  We are currently manufacturing metal materials

  construction (alloys) by melting the metal

  base tal to bring it to the liquid state, by adding additional components to it, the melting process being carried out at the temperature of the entire system, this

  which guarantees complete merger and reconciliation

  of the components (figure 2 a annexed to this de-

  order). When the temperature of the alloy drops

  during cooling and solidification, the solubi-

  The alloy components decrease greatly and, at a certain temperature for each alloy system and composition, the solid phases begin to

  precipitate and grow from the homo-

  gene, in the form of crystals of alloy components

  or, more frequently, in the form of crystals of the compounds

  chemical substances of constituent elements (intermetal phases-

  (Figures 2, b, c annexed to this application).

  During additional cooling, the rest of the melt crystallizes in the form of a solid of

  components located in the base metal (Figure 2, d an-

  attached to this request) The metallic phases

  dant a crystal lattice and properties different from those of the base alloy (matrix) strongly affect

  the properties of the alloy system as a whole.

  The size of the intermetallic phases, which

  pitied during the crystallization process of the alloy, must not exceed fractions of a micron, otherwise the quality of the alloy is strongly affected due to the

  loss of ductility and mechanical strength.

  The solubility of metals and metalloids in the metallic matrix is very strongly limited in the state

  solid, and this factor justifies the severe selection of al-

  commercial bindings and the limit obtained in practice in improving the properties of commercial construction alloys due to a modification of

their composition.

  We have developed a new class of materials

  of construction, which contain, in the incorporated state arti-

  ficially, particles or fibers of oxides,

  carbide and other compounds for obtaining pro-

  guaranteed properties of the system as a whole.

  materials are known to be composite products since the constituents of the metallic system do not precipitate from the matrix metal, as in

  the case of conventional alloys, but are incorporated arti-

  formally in the system All metal alloys

  known representing the matrix with particles incorporated

  whose properties differ greatly from the ma-

  are basically composite products, although they appear naturally in manufacturing

of alloys.

  The properties of metallic materials represented

  felt by a composite system of artificial and natural origin are as follows: the ductility of the material is determined by

  the suitability of the matrix (in general the suitability of solu-

  solid constituents in the base alloy) to have a plastic creep, as well as by the dimensions and the crystal structure of the intermetalloids and other inclusions in the matrix; mechanical strength, resistance to

  heat, resistance to fatigue, resistance of ma-

  The developmental cracks are determined by the interaction of inclusions and the matrix, as well as deformations of the crystal lattice of the matrix under the action of inclusions;

  hardness, wear resistance, pro-

  tribotechnical properties of the material are determined by the properties of the inclusions;

  the modulus of elasticity, the coefficient of dila-

  linear tation, the specific gravity (density) of the material are determined by a set of properties of the matrix

and inclusions.

  This is why the development of new ma-

  metal materials with a predetermined combination of machinability and service characteristics must be able

  be obtained in theory on the basis of the choice of the composition

  optimal metal system in each case,

  that is, the selection of the matrix and the inclusions,

  whose properties and interaction determine the pro-

  properties of the composite system as a whole.

  The selection of the base (matrix) of the mete

  size is determined by required properties of service

  defect in the material and in the level of its properties (steel,

  aluminum, copper, magnesium, nickel, etc.).

  The main difficulty in implementing the

  technology to produce metal materials-

  construction is the injection of constituents into the structure in the form of extremely fine particles of thermodynamically and thermally stable compounds in the matrix, the size of which is understood

  between a few nanometers and a few microns.

  In the manufacture of metallic materials

  natural posites (e.g. complex alloys), the

  problem is solved by means of party precipitation

  cules (intermetalloids) from supersaturated solid solutions of the constituents of the alloy in the metal of

  base, this being produced by the use of a re-

  cooling at high speed of homogeneous melts.

  The required cooling rate can be obtained

  practically only in the case of relative quantities-

  low levels of molten alloys In practice, a degree

  high cooling is obtained by means of a disper-

  physical mass of the melt followed by cooling

  fine drops of the melt in a cooling medium This requires expensive

  drying, degassing and packing of particles (granules

  strips) to obtain pellets This is why, the techno-

  production of new metal alloys in

  using the pelletizing technique has not been very useful

industry.

  The difficulty of introducing extremely small particles

  There are two causes of fine particles in metallic melts. First, due to the lack of fluidity of extremely fine particles (one thousandth of a micron in size or less), the dosage of the particles when injected into the Melt is quite difficult or even sometimes impossible Secondly, due to the presence of oxygen adsorbed on the surface of the particles when they come into contact with the melt, the oxides of the base metal are formed on the surface, which prevents the wetting of particles by the molten mass This problem manifests itself in particular during the injection of

  particles in the molten masses of metals having a re-

  high activity with oxygen (aluminum, magnesium, etc.) The factor indicated above also prevents

  implementation of techniques such as di-

  alloys by injection of particles - crystallization cores in the melt, alloys of the melts by injection of alloy components in the form of a powder, use of waste in the form of powder of alloy materials ( for example silicon) in the manufacture of alloys, in particular those of the aluminum-silicon system. One of the most important characteristics of the proposed technology and of the devices for its implementation is the possibility of injecting into the melt fine particles of filler materials (in the case of the manufacture of composite products) or of structural components. (in the case of the manufacture of alloys),

  by means of the formation of the conformal alloy structure

  ment to the diagram illustrated in FIG. 3, appended to the pre-

feel request.

  Particles of a desired filler material are injected into the matrix free of the atoms of the constituent (FIG. 3 a annexed to the present application) When there is, in the system, a balance between the structural constituent (Ax Py) and the solution of the alloy component P

  in the matrix A, the particles incorporated in the ma-

  dissolve at the saturation concentration at the appropriate temperature with reduction of their dimensions, this process being able to be highly controlled and allowing the manufacture of alloys having a structure with alloy

  with a predetermined constituent having limited solubility

tee.

  The main steps of a process for the fa-

  brication of molded composite materials considered are described in "Solidification, Structures and Properties of

  Cast Metal-Ceramic Particle Composites "Rohatgi P K, As-

  thana R ;, Das S Inst Metal Rev, 1986 Vol 31, N 3 pp 15-139 and include: production of the basic melt; uniform distribution of solid particles in a mass of molten metal;

  crystallization of the resulting composite material

  so much. The methods indicated below have been used in the prior art to inject extremely fine particles into a melt as described in "Cast Aluminum-Graphite Particle Composites a Potential

  Engineering Material "Rohatgi P K, Das S, Dan T K -

  J Inst Eng, March 1989 Vol 67, N 2 pp 77-83: mechanical agitation of the melt and the added particles; pressing the pellets mixed with matrix metals in the powder state and with reinforcing particles, followed by insertion of the particles into

  the melt and mechanical agitation of the latter

  last; dispersion of particles in the melt

  by means of irradiation with ultrasound.

  The problems we encounter in manufacturing

  cation of molded metal composite products,

  lack of wettability or poor wettability

  particles of reinforcing filler with the ground mass

  due constituting the matrix, as well as the non-uniformity of the

  molded material due to significant differences in den-

  between the matrix and the filler material.

  The increase in the mechanical resistance of the bond between the reinforcing filler particles and

  the base metal matrix is obtained by means of a

  any number of techniques as described in "Weta-

  bility of Graphite to Liquid Aluminum and the Effect of alloying Elements on It ", Choh Takao, Kemmel Roland, Oki

  Takeo Z Metallklunde "1987 Vol 78, N 4 pp 286-

  290, i.e.: coating application, wettable by a

  metal, on the surface of the reinforcing filler particles

  is lying; introduction of surfactants into the melt of the base metal; increasing the temperature of the melt. There is also known a process for manufacturing

  composite products (patent application N 51-141960 de-

  posed in Japan on 08 04 80 (NO 55-45955), published 5.11 81), according to which it is suggested to use as filler, hollow natural microscopic beads with a diameter of 150 microns, sufficiently compatible with different materials metallic, as well as graphite powders, Ti B 2, nitride and aluminum oxide, lamellar graphite and in the form of chips and metallic calcium,

  which are added to the melt in an amount

  taken between 0.05 and 5% by weight to guarantee uniformity

formity of materials.

  The main drawback of this process is

  in the need to introduce into the melt an element

  ment (calcium), which is soluble in the base metal li-

  quide, but practically insoluble in the case of a ma-

  solid and which forms a brittle eutectic component

  with the matrix This leads to an alteration of the properties

  mechanical tees of the matrix and of the composite product itself

  even In addition, the use, as a filler, of hollow microscopic beads having the indicated sizes (150 microns) does not contribute to improving the values

  absolute mechanical properties and can lead unique-

  lie to some improvement in their relative values

per unit of mass.

  The prior art relating to the present invention

  is the manufacturing process for composite materials (Met.

  Trans, 1978, v 9 N 3, pp 383-388) which uses metals

  basic molten Mg Al, Fe, Ni, Cr, Co doped with particles

  insoluble oxide cules (A 1203, Be O, Ca O, Ce O 2, Ti O 2, Mg O, Th O 2, VO 2, Zr O 2), carbides, borides, nitrides of Nb, Ta , Hf, Ti, Zr having sizes between 0.01 and 10 microns The particles are injected under the

  powder or thin fiber form To ensure the

  uniform distribution of the particles in the melt, they are injected into a stream of inert gas previously heated (Ar, He) while vigorously stirring the base metal The percentage by volume of the particles can be between 0.5 and 1% of even, one of the elements that improve surface activity at the interface

  particle-melt, is injected into the molten metal.

  The injection of such surface-active metals (Mg, Si, Ti, Zr, V, Nb) guarantees the formation of an envelope, suitable for being wetted by the metal, on the oxides, which greatly improves the wettability in the system and does that there is no segregation in the melt during

a period of 30 minutes.

  The process indicated above presents the in-

  following: 1) the chemical composition of the melt of

  the matrix is limited by the need to inject

  surfactant levels, which in a number of cases

  can lead to a disturbance in the technical properties

  logic and mechanics of the resulting composite material;

  2) the absence of agitation during the solidification

  cation promotes, especially in the case of a long time

  solidification, the formation of segregated and strategic zones

  tified, and therefore the quality of the resulting composite material is reduced; 3) the insolubility of the reinforcing particles excludes the possibility of using this process to manufacture

  materials, the matrix of which is reinforced with par-

  extremely fine particles of these elements or their components

  posed, which are traditional reinforcing agents

  in the manufacture of materials, due to the crystal-

  bonding of base metal joints with additives

  of alloy and subsequent thermomechanical work.

  An object of the present invention is to improve the quality of composite materials by means of a

  increased uniformity of dispersion of parties

  reinforcement load cells and the strength of their ad-

  inheritance in the matrix formed of the base metal, and the ability to produce an expanded group of the composite material through the use of a wide range of ceramic particles,

  of metals and intermetallic products including

  bures, nitrides, borides, oxides, graphite

and glasses.

  The previously stated goal and others are

  achieved through the process of making materials

  posites, characterized in that it includes the stages consis-

  both to entrain particles of solid additives finely

  divided, for example from a ceramic, a metal, a pro-

  intermetallic compound including oxides, borides, carbides, nitrides, graphite, glasses in a gas

  inert and ionize the inert drive gas for heating

  iron the solid particles at a lower elevated temperature

  lower than the temperature at which the particles become

  are not solid due to fusion, sublimation

  or dissociation, but greater than about half

  value of such a temperature, and inject a current from the

  ionized entrainment gas and heated solid particles

  fairies and entrained, in a mass of molten metal, while maintaining a movement of agitation in the mass of the molten metal, sufficient to promote and maintain the dispersion of the particles added so that they solidify under

  the shape of a composite mass, while maintaining a

  agitation in the molten metal containing particles

  solid cules, until its solidification is com-

devotion.

  Other features and advantages of the pre-

  sente invention will emerge from the description given below

  after reference to the accompanying drawings, on the-

which:

  Figures 1, 4 and 5 show arrangements

  for the implementation of different forms of reali-

  sation of the invention; and Figure 2 (2 a, b, c, d) and Figure 3 (3 a, b, c, d), which have already been mentioned, represent

  metallurgical conditions appearing during the formation

mation of an alloy.

  In the practice of the present invention, the melt of the base metal can be aluminum, iron, copper, magnesium, nickel, cobalt, chromium. Suitable base metals are alloys of previously mentioned metals, in which they form the predominant constituent element, such as for example aluminum containing up to 40% by weight of manganese, and steels, and materials such as cast iron and

  modular cast iron Similarly, it should be used as a

  base rates, copper, nickel, titanium and al-

bonding of these metals.

  The addition particles formed by the reinforcing filler are very fine and have an average size of between 1 and 100 microns. The particles can be particles of metals and do not form chemical compounds with the elements of the matrix, such as for example. If in Al; intermetallic products such as: Ti A 13, Zr A 13, Fe Ai 3, Fe 2 Al 5, Cr A 17, Cr A 13, Ni Ai 3, Co 2 A 19, Sc A 13; carbides such as: Si C, Ti C, WC, Nb C, Fe 3 C; nitrides such as Ti N, Si 3 N 4, Zr N; borides such as Ti B 2, Al B 2; oxides such as: Zr O 2, A 1203, Ti C 2, B 203; and also other ceramic materials such

  that sapphire, glasses, graphite and carboni-

  Other particulate materials used to strengthen the dispersion of metals provided

  that they maintain a satisfactory thermodynamic stability

  health during the stages of the present process.

  The inert entraining gases used in the context of the present invention are preferably argon or helium, although other means may be used.

  inert gases The inert gas is ionized and the particles

  trails are previously heated in ionized gas

  before being injected into the melt, at a temperature

  high ture lower than that at which the particles melt or sublime or dissociate, i.e. at a value equal to about 0.9 times the melting point, the

  sublimation temperature or dissociation temperature

  tion, as the case may be At a higher temperature, the

  the particles aggregate to produce particles of a desirable size in the melt, either become particles of a composition other than that desired, or there is a substantial reduction in the desired amount of particles in the melt. particle temperatures below about 0.5 times the melting point (the sublimation temperature or the dissociation temperature), it does not appear in the

  resulting composite product, no increase in

  mechanical strength, hardness and structural uniformity

  turelle, uniformity of dispersed particles and homogeneity.

  The temperature range for pre-heating

  the particle lable has been determined experimentally on the basis of the requirement of obtaining a necessary degree

  and sufficient activation for an action between phase ga-

  rantant a solid bond between the particles and the base metal, due to the withdrawal of the oxygen adsorbed to

  from the surface of the particles, during a corro-

  ion ion and a break in the particles in the

  base current from the surface of the molten metal.

  Determining the appropriate temperature range

  erasures applicable to a particular particulate material can be determined from temperature data published in manuals or the like, and from the use of pyrometric devices, for example sold by

  Agema with an accuracy of 10 C However, it is frequently

  more suitable, especially when using particles such as intermetallic products or

  others and when the published data are not available

  adequately, establish basic conditions.

  For example, before manufacturing the composite products, a test cycle is carried out with the ionization device of the

  gas to be used for the pre-heating stage

  lable, for a particular loading of the particles, and the gas stream, and the residence time of the particles in the ionized gas is increased to the value precisely required to melt (volatilize or dissociate) the particle, the particle is observed and then slightly reduces the residence time to avoid melting etc. These treatment conditions then provide the temperature equal to 0.9

  times the melting point For a residence time equal to

  about half of the residence time, for which the particle melting occurs, corresponds to 0.5 times the point

  We can similarly determine the inter-

  empirical values by adjusting the gas flow and the char-

  management of particles in the gas based on concepts

  fundamentals well known in the art.

* A particular choice of particulate materials-

  ment effective for use in the present invention is listed in Table A indicated below, with the temperature ranges and also indicated base metal compositions taken as

examples.

TABLE A

  Particle Size of Additive, Melt (composition) particles range of basic tem microns peratures C Si C 5-50 1100-2000 Al, Alloys of Ai A 1-4% Cu-1.5% Mg 0, 5% Mn, Fe Ti A 13 1-10 670-1200 Al, Alloys of Al Al-4% Cu-1.5% Mg Ti B 2 5-10 1400-2500 Al, base alloys of Al Si 3 N 4 1-5 950 -1710 Cu, Ni Graphite 5-50 1800-3240 Al-12% Si

  In accordance with the present invention, it is possible to in-

  body about 0.5% by weight and up to about 25% by weight of a filler material in a bath of molten base metal and in the particulate material, and the amount added is determined based on concepts known in the art. the technique for obtaining an improvement or a combination

  particular mechanical properties, for example the

  reté, mechanical strength, ductility, elasticity.

  Table B reproduced below indicates exemplary particle contents and base materials and provides an indication of the improved mechanical properties.

TABLE B

  Particle Quantity Metal of Property (composition)% by weight base (improved com position) 1 Sic 10 Al Rm = 200 M Pa, E = 120 KN

MM 2

K 1

___ = 9

  K 2 2 Zr Al 3 + Cr A 13 1 + 1 Al Ro 2 = 0.99 Rm Ti A 13 15 Al Si = 300 s 3 with Rm temporary tensile strength RO, 2 apparent elastic limit, E modulus d elasticity, K linear wear coefficient, S specific density of particles in the matrix, 1,2,3 indices applicable to a composite material based

  aluminum, aluminum and Al-10% Ti.

  In the practical implementation of the present invention, it is important that the molten base metal is physically active, for example by being continuously subjected to a stirring force from the start of the introduction of the

  solid particles, until the molding and solidi-

  fication of the cast metal are complete Initially, the base melt is physically agitated, i.e. it is located in a crucible-type container and preferably a stirring force is applied appropriately bathing the base metal using non-contact magnetic means, as is known in the art At this stage of the process, one can also

  implement mechanical agitation using ro-

  torsion of known type The degree of agitation must be sufficient

  sufficiently intense, that is to say there must be a continuous observable rotation of the bath, to guarantee a uniform dispersion of the additive particles, and test samples can be taken at intervals to determine this dispersion When the melt of the base metal containing the particles is ready to be molded, the material is transferred directly into a suitable mold and physical agitation of the molten material in the mold is maintained, suitably by means of vibrations, for example at using ultrasonic energy applied to the outside of the mold and causing vibration in the molten metal until all of the metal in the mold has solidified The application of ultrasound to

  getting physical restlessness must be sufficiently

  tense to maintain the uniformity obtained in the crucible,

  but must not lead to significant visible displacement

so much of the mass of molten metal.

  In the practical implementation of the present invention, the stream of ionized inert gas, in which solid particles are entrained, is injected into the bath.

  base metal, so that solid particles penetrate

  trent in the bath to a depth of at least 5 cm, by

  example over about 10% of the depth of the bath. Agitation continues during the change in volume of the liquid phase

  from 100% to 0%, i.e. complete solification, is a prerequisite of the present invention to guarantee a uniform distribution of the reinforcing material in the volume of the matrix, which is allowed by the preceding stages of the process, and improved wettability at the "particle-melt" interface The absence of agitation at any stage of the liquid-solid state of the material

  composite can lead to a weakening of the contact

  between the matrix of the base metal and the parts

  cules, and to the undesirable formation of stratifications, segregations and heterogeneities of the chemical composition

and structural.

  The thermodynamic stability of the particles in the melt of the matrix prevents their chemical action

  with the base metal and the formation of undesirable compounds

  rables with uncontrolled sizes and shapes, which

  rantit, unlike the technology of the prior art,

  the formation of alloys reinforced by extremely small particles

  fine, thanks to the fusion of the base metal, followed by the combination of crystallization and heat treatment, and the manufacture of composite materials of the "metal-intermetallic phase (metal)" type, in which the quantity, the sizes and shapes of the phases of

  reinforcement have preset values.

  With reference to FIG. 1, a crucible 10 suitably made of graphite contains a bath of molten metal 1 formed from the metal of the matrix, for example of

  aluminum, which is stirred by means of a magnetic inductor

  classic tick 4 used to physically stir the metal bath

  size 1, preferably in the rotational movement

  tense illustrated in Figure 1 The crucible 10 has a protective cover 15, in which is installed an ionization chamber 2 having an increased length The inert gas, for example argon, is introduced in a manner which can be controlled at from pipes 8 in an ionization chamber 2, and the gas is ionized so as to produce a plasma arc according to known techniques, and

  in the ionization chamber 2, temperatures appear

  very high tures between 8000 C and 20 000 C Un

  finely divided filler material is retained in the

  crumb 3 with metering means (not shown) used to measure the weight of the finely divided filler material, which is introduced via the conduit 16 into the ionization chamber 2 The filler particles penetrating into the ionization 2 are rapidly heated to an elevated temperature lower than that at which the melting of the particles occurs, for example between 0.5 and

  0.9 times the temperature of the melting point of the particles.

  The particles thus heated and activated, which are

  streaks in a stream of ionized inert gas 25, are in-

  produced in the molten bath 1 by the injection of the inert gas and its penetration below the surface of the bath

  metallic Continuous physical agitation of the metal bath

  lique 1 by the magnetic inductor 4 establishes a uniform dispersion of the particles of the activated and heated solid charge The temperature of the metal bath is measured for example by means of thermocouples (not shown), which makes it possible to ensure that the temperature is less than that at which undesirable melting or decomposition of the filler particles takes place The uniformity of the

  dispersion of the filler particles in the bath is

  blie by means of the analysis of samples taken from the bath at appropriate intervals When the desired quantity

  predetermined solid charge particles has been intro-

  taken from the molten metal bath, the cap 5 located at the base of the crucible 10 is opened, and the molten metal containing the solid particles of additives O is introduced into the

  mold 6, made appropriately for example from steel.

  The molten metal is caused to solidify in the mold and surrounds the solid particles of uniformly dispersed filler To be certain that the solid particles of filler remain uniformly dispersed in the molten metal phase during the progression of the solification, a transducer with ultrasonic 7 is coupled to the mold 5 so that the molten metal located in the mold is physically agitated by ultrasonic vibrations until

  the entire molten phase has passed to the solid state.

  Figure 4 (a) shows the crucible of Figure

  1 fitted with a conduit 20 intended to introduce a reducing agent

  active in the ionization chamber 2 'with an accelerated speed

  flood of the ionized gas indicated at 25 so as to have a

  deeper absorption of the additive in the metal bath

  Figure 4 (B) shows the crucible in Figure

  4 (A), in which the ionized gas and the additive are introduced

  due to the lower part of the crucible The inert gas forms bubbles 30 which burst and are dispersed under the action of an ultrasonic transducer 12 in contact with the upper part of the metal bath at its surface. FIG. 5 represents the crucible of FIG. 4 (B) equipped with the ultrasonic transducer 12, the injection of the

  ionized gas 25 being offset from the center alignment

  tral of Figure 4 (B) so as to obtain the upward helical movement shown bubbles 30 containing particles.

EXAMPLE

  To test the process according to the invention, unalloyed metals, aluminum and iron were used, as well as an aluminum-based alloy, namely 4% Cu, 1.5% Mg,

  0.5% Mn also known under the name D 16 We used

  read these materials separately as a melt of

  basis for producing different composite materials The ma-

  reinforcement materials used initially were

  powdered silicon bure, size 5-50 microns, aluminum

  titanium miniure Ti A 13 with particles with a size of 1-10 microns, and also titanium powder with

  particles with a size of 10-100 microns.

  Tests were carried out to produce a composite material in the pilot unit shown diagrammatically in FIG. 1 The crucible was made of graphite and

  contained a melt 1 forming a matrix, which was in-

  jetted with a stream of ionized argon gas which entrained reinforcing particles previously heated to a predetermined temperature using a device

  classic ionization type plasmatron 2 equipped with the dis-

  positive fusion 3 to obtain a predetermined flow of

  circulation of the powder in the ionization device.

  The temperature of the Tp particles was modified and it was checked by detecting the variation in the net content of the

  basic melt before and after the injection of parti-

  powder particles Tp was calculated in accordance with the

  mule: Cm Mm Tm (1 + KN) Tp = (1 to with Cp Mp e 0 temperature of the melt after injection of the additives, 'C;

  Tm matrix temperature before injection of additives

tifs, OC.

  Cm specific value of the metal forming the matrix, Mm metallic mass, Kg, C specific heat of the particles, Mm Mass of the particles, kg, Kn dimensionless factor taking into account the effects

  thermal during air cooling of the over-

  face of the melt during reheating during

  treatment with a stream of ionized gas without

  particle junction, Kn = 0.05-0.06 for 5 kg of molten metal and a flow of ionized argon gas of

0.1 m 3 / min.

  The mixture was stirred during molding with injection of additives by means of the magnetic inductor 4 After injection of predetermined quantities of solid additives, the plug (5) was removed from the crucible and the liquid-solid mixture in the hole at the bottom of the crucible to fill a mold made of steel The steel mold (6) with a diameter of 50 mm was used and the mixture of molten metal and solid particles was stirred using an ultrasonic generator 7 until the contents of the mold are solidified The solid molded mass obtained was 2.5 kg hot extruded The quality control of the resulting composite material was determined on the basis of the following parameters uniformity chemical and structural, size of the reinforcing particles,

  mechanical resistance of the composite material.

  The chemical heterogeneity of the composite material was evaluated by modifying the content of constituents formed

  reinforcing particles in different cross sections

  versals of the molded part, across the direction of casting, by means of the determination of the chemical heterogeneity factor K Cmax Cmin Kc = 1 n 1 Ck nk = 1 with Ck content of constituents formed of reinforcing particles in the section cross-section of the molded part,% by weight n number of cross-sections analyzed; Cmax, Cmin maximum and minimum contents of the constituents formed of the reinforcement particles in the

cross sections,% by weight.

  The structural heterogeneity of the composite material was determined by modifying the average sizes of the reinforcing particles, using the factor Kave Kav = -max din 1 n X di n i = 1 with

  di mean size of the i-th particle, in mid

  crons; dmaxi dmin maximum and minimum sizes of the particles analyzed,

n number of particles analyzed.

  The mechanical strength was determined in

  the tensile strength Rm, in M Pa (UTS) The chemical composition was determined using the ARL 72000 quantimetric measuring device, with an accuracy of + 0.01%; the structural characteristics were determined using the Me F-3 A metallographic optical microscope with magnifications up to 3000 X, and with the Omnimet 2 structural analyzer for the quantitative determination of the elements contained in the structure Determination of the resistance mechanical work was carried out by the UTS-100 tensioning machine with a maximum applied force of 100 k N All of the above equipment is part of the state of the art The table

  1, reproduced at the end of the description, indicates the results

test states.

  Evidence shows that the best

  characteristics are guaranteed by the samples of ma-

  composite materials manufactured during experiments N 06, 9,

  12, 36, 42, 51, 57, 66, 69, 72 in accordance with the se-

  lon the present invention for manufacturing the materials

metal based posites.

  In another embodiment of the pre-

  invention, the filler material for manufacturing a composite material is synthesized in the environment of an ionized entraining gas and the nascent materials thus

  obtained, protected by ionized cleaning gas, are

  products in the melt of the base metal, which is

  physically agitated, for example using mat techniques

  genetic or ultrasonic techniques so as to repair

  uniformly firing the synthesized material in the matrix of the base metal The filler materials are synthesized by the introduction of substantially stoichiometric quantities of the reagents used to produce the filler material For example, during the manufacture of the nitride filler material titanium, titanium powder having appropriate sizes between 20 and 50 microns,

  is entrained in nitrogen gas in correct proportions

  corresponding to the equation: 2 Ti + N 2> 2 Ti N The titanium / nitrogen mixture is introduced into a flow of ionized inert gas and is exposed to the ionized gas at a temperature in the range between 2200 and 30000 C for a sufficient time for the reaction to be complete between titanium and nitrogen to form titanium nitride in the vapor state, which is entrained by the ionized inert gas on the surface of the base metal melt , for example aluminum,

  and is physically agitated so as to disperse uniformly-

  the titanium level in small discrete volumes

  which, upon solidification in the base metal, provides

  particles of extremely reinforcing filler

  The other filler materials can be synthesized similarly as follows 3 Si (powder) + 2 N 2> Si 3 N 4 Ti (powder) + 3 Al (powder)> Ti Al 3 The temperature of the mass base metal melt is maintained at a value which causes quenching of

  additive materials so that the additive material synthesizes

  is not dissociated, undesirably, in the

melt.

  In another embodiment of

  the invention, a gas containing carbon, such as hy-

  drocarbons, propane, butane natural gas, methane or carbon monoxide and carbon dioxide are ionized in the mixture with a stream of ionized inert gas and are dissociated The carbon dissociation product is the mono-atomic elemental carbon, which is injected into the basic melt as an additive filler For

  gases containing oxygen, mono-atomic oxygen li-

  béré is a stream of ionized gas which reacts with the molten mass, for example formed of aluminum, to form particles of extremely fine charge of aluminum oxide

A 1203 in the melt.

  After the practical implementation of the present invention under the conditions of Table 2 and by means of the use of the materials of this Table 2, the additives indicated were introduced into the base molten metal matrix indicated to obtain composite materials having

  improved mechanical properties.

Claims (60)

  1 Process for manufacturing a composite material, characterized in that it consists in entraining particles of a finely divided solid additive, in a stream of ionized inert gas and in ionizing the inert gas and using the   heat produced by the ionized gas to heat the parts   solid cells at a high temperature below the time   temperature at which solid particles become non-solid under the effect of fusion, sublimation or   dissociation, but greater than about half   value of such a melting, sublimation or dissociation temperature, and injecting said gas stream and the heated heated solid particles into a mass of molten metal to obtain a mixture of solid particles   finely divided and molten metal and then produce a   physical ration of the mixture of molten metal and solid particles to obtain a substantially uniform distribution of solid particles in the molten metal, and continue   physical agitation of the molten metal until the   mixture of finely divided particles and metal either completely solidified.   2 Method according to claim 1, characterized   in that the mixture of the molten metal and the particles   lides is initially contained in a crucible (10) and that the stirring is carried out using magnetic means (4) located outside the crucible, and that later part of said mixture is transferred into a mold (6 ) and that agitation of the mixture is produced by means   ultrasound (7), located outside the mold.   3 Process for manufacturing a composite material,   characterized in that it consists in entraining, in a cou-   rant of ionized inert gas, a finely dispersed solid reagent   target and / or a gaseous reagent in proportions allowing   to obtain, during the reaction, a predetermined composition   born, cause a reaction between said reactive products while they are entrained in said ionized inert gas   to obtain a reaction product intended to be introduced   duit in a molten metal bath (1), and causing physical agitation of said metal bath to uniformly disperse said reaction product in this bath. 4 Method according to claim 1, characterized in that said base metal is chosen from aluminum, iron, magnesium, copper, nickel, chromium, titanium and that said additive material is selected from chemical compounds , comprising two or more compounds, from one of the base metals with other metals, as well as from carbides, nitrides, carbonitrides, oxides and metal borides.  5 Composite material or alloy containing uniformly distributed components, characterized in that it is formed by injecting additive particles which have been heated by an ionized gas, in a physically stirred molten base metal, the material obtained being removed in continuous injection area, with cooling   while continuously maintaining physical agitation if that.   6 Composite material or alloy according to resale   dication 5, characterized in that said base metal is chosen from aluminum, iron, magnesium, copper,   nickel, chromium, titanium and that said additive material   tif is selected from chemical compounds,   two or more base metal compounds with other metals, as well as carbides, nitrides, carbonitrides, oxides and borides of metals.   7 Device for manufacturing a composite material   site, characterized in that it comprises: (i) crucible-shaped means (10) intended to contain a molten base metal; (ii) means (2) for producing a plasma arranged in the vicinity of the crucible-shaped means (10) for receiving a stream of inert gas and particles of entrained charge and for ionizing said gas and heating it makes said particles; (iii) means (2) for injecting said ionized gas and the heated particles into said crucible-shaped means (10) so that they penetrate the molten metal when the latter is present in said crucible; (iv) means (4) for continuously agitating the molten metal when it is present in said crucible; (v) mold means (6) for receiving the molten metal containing the filler particles from said crucible; and (vi) means (7) for continuously agitating the molten metal when it is present in said mold means.   8 Device according to claim 7, character-   laughed in that said crucible (10) is covered with a cover (15) and that the means (2) serving to inject the ionized gas and the heated particles pass through said cover.   9 Device according to claim 7, character-   laughed in that the means (4) used to stir the molten metal in the crucible (10) are magnetic stirring means.   Device according to claim 7, character-   laughed in that the means (7) for stirring the molten metal in the mold means (6) are means form of ultrasonic transducer.   11 Device according to claim 7, character-   risé in that the means (2) for injecting the ionized gas and the heated particles cross the bottom of said crucible (10).   12 Device according to claim 11, charac-   characterized in that said ultrasonic transducer means (7) are provided in the vicinity of the part   upper crucible means (10).   13 Device according to claim 12, characterized in that the ultrasonic transducer (7) and the means (2) for injecting the ionized gas and the heated particles are moved horizontally so that the molten metal located in the crucible ( 10) is trained in rotation. TABLE 1 Test results temple-   erasure of the matrix 0 oe material of the temperature matrix. type of reheating material   of reinforcement of golden powder necessarily modify cation sition from the from the- quantity quantity of the compound phase 11 Fie? W / site medium size some-   reinforcement microns k c k Rm ave M Pa * NVL 2 7 ua 9 O I 2 3 4 5 6 Ull 10 0.14 O 12 67 (TO AI 11 0 11 mt W # 08 0 10 W w O 09 02 O 08 208 SIC 880 # NOT w Flow of left-   cules / Flow of inert gas Mn / Mn NO of laa. o. 0. O il Ai-SIC -80 -0 -0 10 -0 -0 -80 -0 -0 -80 -0 -0 -80 -0 -0 O 5 O 6 O 4 a O 4 at 0 5 O 0 1 7 0 4 7 O 5 7 0 08 6 0 4 6 0 5 6 0 07 0 3 1 S 0 4 0 18 0: 3 2.2 160 2.2 150 2.2 180 0.8 215 0.8 205 - 0.8 '250 0.7 220 0.7 210 0.7 255 0.5 225 220 0.5 260 3,195 4,190 2,200 K, (O 0 o FD L 2 3 4 5 6 7 8 9 10 16 O 15 17 n 18 l 19 0 12 22 0 9 0 6 26 I 27 n 28 0 3 I 31 0 18 32 n 33 n 4 O 15 '' 36 # 0.12 A 1 t n n O 0.11 " n n 0.10 n n n n 0.9 n n fn n n 0.8 I   n n n n 0.12 n n n 0.11 n n nf t, n Al-Ti-Ti A 13 n n of Il n n n n IN t, Al-Ti Als e 'n t' II i ' 0 4 0 5 0 3 0 4 O 5 0 3 0 4 O 5 0 3 0 3 0 4 0 2 0 2 O 3 0 15 7 0 3 7 0 6 7 0 4 4 0 4 4 0 6 4 0 6   nnn ft nnn N nn le n of nn In tnt,% Ti It tf n Il nnnnnnn% Ti A 11 nnn II Il I Il nnnn # nnt I le n ni Ut -95 -0 -0 -95 -0 -0 -95 -0 -0 -95 -0 -0 -95 -0 -0 -85 -0 -0 -85 -0 -0 a 8 0.8 0.6 0.5 Ni o) FD 1 2 3 4 5 6 7 8 9 10 37 0 12 38 n 39 n 0 09 41 n 42 X n 43 0 06 44 n I 46 O 14 47 " 48 I 49 O 11 e, e 52 0 08 53 rd 54 " '0 05 56 i 57 O #   0.10 A 1 670 15% Ti A 13 n N n # Il O 'f Il 0.09 Il' Of 0.08 "N"   le I N n 0.12 D 16 660 20% Si C I * N Il gg go 0.11 et 0.10 'l 0.09 N 9   te UI Il a Ig * l O te O te O n rtg ne Io es el It n Il # n le fi n il te el le le -85 -OT -0 -85 -0 -0 -85 -0 -0 -80 -0 -0 -80 - 0 -0 -80 -0 -0 -80 -0 -0 A 1-Ti All 3 n 3 n 3 I O 2   n 2 2 2 n 15 "20 n 10 D 16-if C 20 n 20" 8 "8 n 7 O 7   n 7 e 6 "6 n 6 0.3 0.4 0.05 0.2 0.3 0.05 0.2 0.3 0.1 0.4 0.5 0.3 0.3 0.4 0.09 0.3 0.4 0.07 0.3 0.4 0.05 0.6 0.6 0.6 0. 4 0.4 0.4 0.7 0.7 0.7 0.6 0.6 0.6 0.5 0.5 0.5 w CD 0 ' ) 0 '0' O 3 w D 1 2 3 4 5 6 7 8 9 10 0.08 D 16 660   Il N n Hs N n 0.12 Fe 1540 n N n n N n 0.11 N n n N n n, N n 0. 10 N Il n N n n n, n #f Il It 0. 09 l u ns N n o, N n 0.08 "   e N n II It,% Sic% sic Il ui It and el el il and O f If nn 1100 oo nnnno '-80 -0 -0 -80 -2 -0 -80 -0 -0 -80 -0 -0 -80 -0 -0 - 80 -0 -0 D 16-sic 15 "1 15 "15   Fe-Si C 20 n 20 n 20 n 8 n 8 n 8 n 7 n 7 I '6 n I 6 # 6 i 15' ii 15 0.2 0.3 0.09 0.6 0.7 0.5 0.5 0.6 0.12 0. 4 0.6 0.10 0.3 0.5 0.8 0.4 0.5 0.1 2.5 410 3,400 1.5 420 2.5 620 2.5 600 2.5 650 0.9 690 0.9 680 0.9 790 0.8 710 0.8 700 0.08 800 0.7 720 0.7 700 0.7 810 3.5 610 4,600 2.5 640   69 '. '0.02 fi n 0.14 n lu 0.11 n 0.08 It le 0.05 os It l 0.02 n lu and w -à t Oi O' (O a b TABLE 2   flow rate of ionized gas (standard cubic feet per minute) & temperature o C amount of addition% by weight device fig 4 (B) fig 5 addition A 1 670 5-50 microns 0.02 kg / mh Ti -50 microns 0.04 kg / m. 14000 Ti A 13 14000 Si 3 N 4 2 + TO +   1540 Ti -50 micron S 0.04 kg / mn Ti -50 min 0.04 kg / mn co 2 14000 Ti C 0.013 M 3 / mn N 2 0.005 M 3 / m n 14000 Ti N metal of the ma- trice, kg temple-   rature of the matrix o C Reactive agent Reactive agent Ai 4.22 kg Cu 4. 9 kg +   If -50 microns 0.02 kg / min N 2 + 0.008 M 3 / one Fe 4.75 Ai 12% if 4.9 + 4- w t LO 2 + K, (O