EP2571653A1 - Procédé de fabrication d'une tôle composite métallique multicouche en utilisant une suspension de particules; tôle composite correspondante - Google Patents

Procédé de fabrication d'une tôle composite métallique multicouche en utilisant une suspension de particules; tôle composite correspondante

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Publication number
EP2571653A1
EP2571653A1 EP11727639A EP11727639A EP2571653A1 EP 2571653 A1 EP2571653 A1 EP 2571653A1 EP 11727639 A EP11727639 A EP 11727639A EP 11727639 A EP11727639 A EP 11727639A EP 2571653 A1 EP2571653 A1 EP 2571653A1
Authority
EP
European Patent Office
Prior art keywords
particles
suspension
sheets
sheet
composite sheet
Prior art date
Legal status (The legal status 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 status listed.)
Withdrawn
Application number
EP11727639A
Other languages
German (de)
English (en)
Inventor
Christian Werner Schmidt
Mathias GÖKEN
Heinz Werner HÖPPEL
Verena Maier
Wolfgang Peukert
Catharina Knieke
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Friedrich Alexander Univeritaet Erlangen Nuernberg FAU
Original Assignee
Friedrich Alexander Univeritaet Erlangen Nuernberg FAU
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 Friedrich Alexander Univeritaet Erlangen Nuernberg FAU filed Critical Friedrich Alexander Univeritaet Erlangen Nuernberg FAU
Publication of EP2571653A1 publication Critical patent/EP2571653A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
    • B23K20/04—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating by means of a rolling mill
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
    • B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K2101/00—Articles made by soldering, welding or cutting
    • B23K2101/18—Sheet panels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K2103/00—Materials to be soldered, welded or cut
    • B23K2103/16—Composite materials, e.g. fibre reinforced

Definitions

  • the invention relates to a method for producing a multilayer metal composite sheet by joining surface-coated partial sheets, comprising the following method steps: coating a surface of a first partial sheet by applying particles, stacking the first partial sheet with the coated surface on a surface of a second partial sheet, joining the Partial sheets by roll cladding including the deposited particles to a first composite sheet, and optionally a repetition of the aforementioned steps using the first composite sheet as a partial sheet to form a composite sheet of a plurality of partial sheets. Furthermore, the invention relates to a composite sheet, which is produced by means of the aforementioned method.
  • Such a method is known as a cumulative rolling process or as a so-called Accumulative Roll Bonding (ARB) method.
  • ARB Accumulative Roll Bonding
  • the basic technology of the ARB process is based on the process of roll-plating sheets to produce a homogeneous multilayer composite from a plurality of partial sheets.
  • the ARB process belongs to the Severe Plastic Deformation (SPD) process and offers the possibility of introducing extremely high deformations into metallic materials.
  • SPD Severe Plastic Deformation
  • an improvement of the material properties of the resulting composite sheets can be achieved by an additional introduction of selected particles on the surface of partial sheets to be joined together.
  • CONFIRMATION COPY have chanical and / or additional functional properties, as the starting materials.
  • surface ultrafine-grained or nanocrystalline materials allow the production of weight-reduced structural components, especially for industrial applications.
  • the UFG materials have good forming properties, as they are necessary in particular in vehicle construction, systems engineering and the aerospace industry.
  • the ARB process can be relatively easily integrated into existing process chains, it also represents a technologically promising method for the production of composite sheets with great lightweight potential.
  • WO 2009/079700 A1 discloses the production of ultrafine-grained materials by means of an ARB process. For this purpose, a uniformly distributed particle layer is applied to the surface of one or two sheets and the sheets are then brought together with the coated surfaces and bonded together. The particles are pressed into the surfaces by creating a reduction in thickness and embedded there. With regard to the type of application of the particle layer, no details are given in WO 2009/079700 A1.
  • a second object of the invention is to provide a composite sheet which has improved mechanical and / or functional properties over composite sheets of the prior art.
  • the first object of the invention is achieved by a method with the feature combination according to claim 1.
  • the method for producing a multi-layer metal composite sheet comprises the following method steps: coating a surface of a first partial sheet by applying particles, stacking the first partial sheet with the coated surface on a surface of a second partial sheet, joining the partial sheets by roll-cladding including the applied particles to a first composite sheet, and optionally repeating the above steps using the first composite sheet as a part sheet to form a composite sheet of a plurality of partial sheets.
  • the invention takes into account that the demands on composite sheets with respect to their load capacity and stress steadily increase.
  • the composite sheets should be structurally and functionally versatile and also be manufactured with low technological effort.
  • the invention recognizes that a defined surface layer is decisive for the desired mechanical and / or functional properties of the composite sheet.
  • the conventional methods basically offer the possibility of influencing the properties of a composite sheet by introducing particles, a controlled application in terms of particle distribution in the sheet plane and dispersity of the particles to form a reproducible homogeneous or deliberately graded particle layer, but is not feasible.
  • the invention solves this problem by the fact that the particles are applied during the process of a suspension on the surface of a partial sheet.
  • the material properties of the composite sheet can be specifically influenced.
  • an ultrafine-grained or nanocrystalline composite sheet can be produced, the properties of which can be adjusted in a targeted manner and which, as a result, are suitable for a wide range of applications.
  • a suspension makes it possible to influence the particle properties by selecting the solvent.
  • a suspension in particular the agglomeration behavior of the particles can be controlled.
  • the surface of the particles can be chemically and electrically influenced, whereby the connection of the particles to the metal matrix within the composite sheet is controllable. Due to the production process of the suspension, the surface of the particles is mechanically manipulatable. In particular, the shape and the surface roughness of the particles can be adjusted, which in turn can influence the binding of the particles to the metal matrix.
  • the controlled application of the suspension additionally allows a targeted grading of the composite metal sheets, whereby targeted and local mechanical and / or functional properties can be set.
  • various solvents can be used, wherein a certain concentration of particles is contained in the suspension.
  • the particles may have different diameters, shapes and surface finishes.
  • the application of the particles for coating the surface can in particular be carried out by known standard methods, which enable a fast and automated distribution of the particles on the surface. In this case, for example, spraying or dipping methods are conceivable which offer the possibility of applying the particles, which are finely distributed in a suspension, to the surface.
  • a film consisting of particles and solvent forms on the surface.
  • the solvent evaporates or evaporates, either with or without heating of the composite sheet, and the remaining particles can adhere to the surface.
  • the particles may be formed for example as a closed particle layer or in the form of a non-closed particle layer on the surface.
  • the formation of both a particle layer or particle layer on the surface here depends in particular on the chosen coating method and its relevant parameters, such as a subsequent heat treatment, the solvent and the concentration of the particles in the suspension.
  • the gradation of a particle layer can be controlled.
  • a thicker coating can be achieved, for example, by repeated multiple spraying on the desired areas to be coated. For example, further areas may remain entirely without surface coating or be provided with only a thin layer.
  • stepless gradients can also be generated by stepless control of the spraying distance or of the volume flow.
  • the use of a suspension to coat a surface during an ARB process provides a particularly easy-to-handle means of controllably controlling a particle layer on a surface Apply and thus to improve the properties of the composite sheet produced targeted or change.
  • first partial sheet is first coated by applying particles from the suspension.
  • the first part sheet is applied with its coated surface on the surface of a second part sheet.
  • the surface of the second partial sheet may also be coated. Both partial sheets are joined together to form a first composite sheet by roll-cladding, including the applied particles.
  • the part-plates are plastically deformed and permanently joined, in particular by roller pressure.
  • the partial sheets are cold-welded together, so to speak.
  • a particle is applied to the surface of one or more partial sheets, the particles are trapped between partial sheets of the composite sheet.
  • the foregoing steps may be repeated until the desired structure and properties, such as increased tensile strength of the composite sheet, are achieved.
  • the first composite sheet obtained after the first pass can be used as a partial sheet for forming a composite sheet of a plurality of partial sheets.
  • sheets are particularly suitable thin metal sheets and foils, for example, aluminum, magnesium, titanium, iron / steel or copper.
  • a thin metal sheet and foils for example, aluminum, magnesium, titanium, iron / steel or copper.
  • either partial sheets of the pure elements or of alloys containing at least one of the elements can be used.
  • Sheets made of these These metallic materials are lightweight, easy to process and easily deformed.
  • the first composite sheet is divided into a number of partial sheets after roll-plating.
  • the partial sheets can be coated once more and returned to the ARB process. Since the composite sheet is already provided with at least one particle layer, the desired properties, such as, for example, the increase in strength and the formation of an ultrafine-grained or nanocrystalline structure, can be achieved particularly quickly by additional local plastic deformation.
  • metallic particles are applied from the suspension as particles.
  • the metals aluminum, titanium, copper and / or magnesium are preferred for this purpose.
  • Such particles are on the one hand due to their hardness to increase the strength of a composite sheet.
  • the introduction of metallic particles allows the electrical and thermal conductivity to be adjusted in a targeted manner.
  • the formation of mixed crystals and intermetallic phases can be made possible.
  • This provides further options for the targeted structure and property settings. It is fundamentally possible to apply different particles to a common surface or to provide a plurality of partial plates with different particle layers and then to join these partial plates together by roll-plating. As a result, the properties of the composite sheet are variably adjustable. For the particles and alloys of different metals can be used.
  • non-metallic inorganic particles are applied from the suspension.
  • ceramic particles may in particular increase the strength and temperature resistance of the composite sheet, improve the tribological properties, and increase the development of the microstructure during the ARB process by additional localization. accelerate kale plastic deformation.
  • electrical or other functional properties of non-metallic-inorganic materials such as the storage and release of hydrogen or the like can be exploited.
  • defined electro-physical and / or electro-mechanical properties can be achieved, for example, by using ceramic nanoparticles.
  • structures can additionally be deliberately introduced into the composite sheets.
  • a graded distribution of the amount of particles over the surface of the partial sheet graded properties can be caused in the composite sheet.
  • the gradation is adjustable on the one hand by the coating process within the sheet plane and on the other hand by a targeted variation of the stacking sequence of different types of sheet metal perpendicular to the sheet plane.
  • a combination of the gradation in the roll plane and a variation of the stacking sequence of the Operabelche in roll cladding and a three-dimensional graded structure can be generated.
  • the areas on the surface can be sprayed several times, where a thicker coating is desired.
  • Other sites can either be thin coated or completely uncoated, which can produce different local properties.
  • a functionalization of the particle layers is possible. This can be achieved for example by particle layers having different electrical and thermal conductivities. This par Particles of different conductivities can be applied either together in one layer or in separate layers. The properties of the composite sheet are thus very specifically controllable.
  • the method allows independent grading of the composite sheet. It offers the possibility of producing a gradation in the rolling plane and thus, in combination with variations of the stacking sequence, also to produce a three-dimensional graded structure. Even a gradation perpendicular to the rolling plane is possible.
  • a functionalization of the composite sheets as well as the mechanical properties with regard to structural use can be combined here. For example, tribologically or fracture toughness-optimized as well as more rigid composite sheets can be produced by grading or also by the combination of functionalization and improvement of the mechanical properties.
  • metal oxides are preferably applied from the suspension as particles, in particular Al 2 O 3 and / or Sn 2 O 2 and / or ZrO 2. These metal oxides are distinguished in particular by their chemical resistance and their resistance to mechanical influences. AI2O3 is also a good insulator and has a high dielectric strength. Thus, by the targeted use of a metal oxide, the properties of a composite sheet can be influenced. A combination of different oxides in a composite sheet is possible here.
  • carbides in particular SiC
  • Carbides have very strong covalent bonds associated with a crystal structure, resulting in high mechanical stability.
  • SiC has a high hardness and is thermally and chemically resistant.
  • SiC has a good thermal conductivity and is relatively resistant to oxidation even at temperatures above 800 ° C.
  • a SiC-containing Particle layer By the application of a SiC-containing Particle layer on the surface can thus be obtained a solid and temperature-resistant composite sheet.
  • a composite sheet having a SiC coating may have different conductivities depending on the temperature. Accordingly, a variety of applications of a SiC particle-coated composite sheet is possible.
  • further carbides for example boron carbide or calcium carbide, which have high mechanical and thermal stability.
  • hydrides particles from the suspension in particular T1H2 and / or MgH.
  • 2 Hydrides act as blowing agents and release hydrogen when the temperature rises, whereby a metal foam is produced from the composite sheet.
  • Metal foams have a low density due to pores and voids, but have a high specific rigidity and specific strength, so that they are suitable for the production of weight-reduced workpieces with high mechanical strength.
  • Even when using hydrides a targeted grading or local introduction can take place, whereby it is possible to produce graded foams or locally foamed composite sheets.
  • particles having an average diameter between 1 nm and 10 ⁇ m are applied.
  • the particle size has an influence on the properties of the composite sheets resulting after roll-plating.
  • increased strength can be observed over a composite sheet having significantly smaller or larger particles.
  • this effect is not only dependent on the size of the particles applied, but also on the nature of the particles and the material of the partial sheet.
  • the material properties can thus be such as the tensile strength can be influenced.
  • the resulting composite sheet preferably has an increased tensile strength compared to the starting material.
  • the tensile strength describes the resistance of a material, ie the composite sheet, in the action of tensile forces. It is usually stated as a stress, that is, as the force acting on a surface.
  • a particle layer having a thickness between 1 nm and 100 ⁇ m is deposited on the surface from the suspension.
  • the thickness depends on the size, ie on the average diameter of the particles applied from a suspension.
  • the coating process such as a spraying process or immersion of the partial sheet in the suspension, and the relevant parameters of the respective coating process, such as duration, concentration of the suspension, etc. may also play a role.
  • the smaller the mean diameter of the particles the lower the layer thickness of the particle layer can be formed.
  • the bond between two partial sheets is usually more pronounced after roll-bonding than with thick particle layers.
  • the thickness of the layer can be adjusted according to the requirements, ie in particular according to the later field of application. This can be done in addition to the choice of the size of the particles, for example, by the targeted reduction in thickness in roll cladding.
  • the particles are stabilized in the suspension prior to application electrostatically or sterically or electrosterically. Due to the various stabilization mechanisms, the dispersity of the particles in the suspension can be adjusted. In this way, preferably the agglomeration behavior can be controlled and a basically disturbing agglomeration of the particles can be prevented. This is possible by increasing the distance of the particles from each other, in particular three stabilization mechanisms are known.
  • electrostatic stabilization the surface of the particles to be stabilized is charged with charges of the same name, so that the particles repel through the Coulomb interaction.
  • Suitable stabilizing substances here are, for example, nitric acid for particles of aluminum oxide (Al 2 O 3 ) or of zirconium oxide (ZrO 2) or ammonia for particles of silicon carbide (SiC).
  • steric stabilization the influence of the spatial extent of a molecule is used.
  • the surfaces of sterically stabilized particles are, for example, coated with macromolecules, such as polymers, which protrude into the solution and thus define a minimum distance between the particles.
  • macromolecules such as polymers
  • PS polystyrene
  • PVP polyvinylpyrrolidone
  • block copolymers such as poloaxamers. These copolymers contain, in addition to the insoluble in the solvent segments, the so-called anchor groups, and segments that dissolve well in the solvent and thus protrude far into this and thus stabilize.
  • Electrosteric stabilization combines both mechanisms.
  • the electrical charges which are responsible for the electrostatic repulsion are located, for example, at the end of the shell of the macromolecules projecting into the solvent.
  • electrosteric stabilization depending on the degree of dissociation in the particular solvent, for example polyvinyl alcohol (PVA), polyacrylate acid (PA) or polyethylene glycol (PEG) can be used.
  • PVA polyvinyl alcohol
  • PA polyacrylate acid
  • PEG polyethylene glycol
  • various liquids can be used as solvents for the particles in the suspension.
  • a suspension comprising a polar solvent such as water or an alcohol such as ethanol.
  • solvents for example, organic acids, ketones, aldehydes, glycols, amides or urea compounds are conceivable.
  • the suspension may further comprise in particular a solvent which conforms to the surface properties of the Substrate, ie in particular a partial sheet to be coated, and having adapted to the surface properties of the particles surface tension.
  • a suspension is used in which the particles are present in a concentration range of up to 40% by weight, in particular between 1 and 5% by weight.
  • the concentration is accordingly dependent on the weight and, taking into account the density of the particles, also of their size.
  • the concentration of the suspension from which the particles are applied can be adjusted.
  • the deposited amount of particles on the surface and thus also the volume fraction after completion of the process can be controlled in the composite sheet.
  • the volume fraction of the particles in the resulting composite sheet may vary depending on the concentration of the particles in the suspension and the number of cycles of coating operations.
  • the volume fraction of the particles also depends on the volume of suspension applied per step. Own measurements have shown that in particular a low volume fraction of less than 0.5% by volume of nanoscale Al 2 O 3 particles results in an increase in tensile strength of up to 20% compared to a composite sheet produced identically by the ARB process without introduced particle layers.
  • the small particle fraction based on the total volume, further shows that the solidification produced by the material introduction occurs even at low volume fractions. Thus, no relevant change in the physical density of the sheet is caused.
  • the increase in the tensile strength is accordingly preferably identical to the increase in the specific strength, ie the tensile strength based on the density of the material.
  • the suspension is prepared by means of a stirred ball mill.
  • Agitator ball mills are preferably used for fine crushing of solids in a suspension.
  • suspensions can be processed directly here without intermediate steps. Concentrating, suspending Ren, dispersing or a solvent change may be omitted.
  • Agitator ball mills can grind substances of different hardness depending on the material of the grinding media and furthermore enable thorough mixing or a homogeneous distribution of the particles in the suspension. In this case, the particles are comminuted by pressure and shear forces between grinding media or between grinding media and Mahlraumgephaseuse and evenly distributed in the solvent. The particle size achieved depends essentially on the mass-specific energy input and on the size of the grinding media.
  • yttrium-stabilized zirconium dioxide or silicon carbide can be used as grinding media.
  • the lower limit of the particle size or the particle diameter to be achieved with a stirred ball mill is usually in a range between 5 nm and 10 nm.
  • the or each surface of the partial sheets is cleaned prior to coating by means of a liquid and / or mechanically surface-treated.
  • a liquid in particular acetone can be used to remove surface dirt or for degreasing.
  • the surface of a partial sheet can be treated mechanically, preferably with a wire brush, before coating with particles. The brushing by means of a wire brush is used to eliminate and break up unwanted surface oxides and to produce a corresponding roughened surface. In this way, a good adhesion of the particles can be ensured before coating on the one hand, and on the other hand the metal-metal contact to a second partial sheet can be improved, so that the binding of two mutually fixed partial sheets can be improved.
  • a metallic material selected from the group consisting of aluminum, titanium, copper, magnesium and iron is used as the starting material for the partial sheets.
  • a pure metal or an alloy is possible.
  • thin metallic ones are suitable Sheets or foils which can be stacked on one another and joined together by roll-cladding.
  • aluminum is suitable because of the good workability and the low density. Aluminum is extremely elastic and can be processed very well into thin films. Due to its low density, aluminum is often used in areas where light weight components are desired, such as aerospace or automotive. Furthermore, very high specific strengths can be achieved by alloying aluminum with magnesium, silicon and / or other metals. Titanium is also suitable because of its low density and has a high melting point as well as a high mechanical strength.
  • titanium is particularly corrosion resistant and has a low thermal expansion coefficient. Accordingly, titanium is particularly suitable for use in thermally stressed areas. Copper is tough and ductile and can also be easily processed into films. Furthermore, copper is particularly conductive. Magnesium and iron are also advantageous as materials for the partial sheets.
  • the partial sheets are subjected to the coating of a surface of a temperature treatment.
  • the solvent evaporates in order to prevent moisture from being trapped inside the metal.
  • the heat treatment increases the ductility of the composite sheet, resulting in improved bonding performance and increased bond strength.
  • a temperature treatment can be carried out after each process run. In particular, relatively low temperatures between 100 and 300 ° C are advantageous depending on the material.
  • the composite sheet is finally heat treated.
  • the composite sheet is preferably heat treated just above the melting point.
  • the heat treatment can specifically target the microstructure and the mechanical and / or functional properties of the process. bundblechs are influenced, and phase formation or solid solution hardening processes are stimulated.
  • particular properties of the incorporated particles such as the storage and release of hydrogen in metal hydrides, can be used to enhance or otherwise provide new or improved material properties of the composite sheet.
  • the thickness of the partial sheets is reduced by 30-80% by the roll cladding.
  • the thickness reduction is dependent on the strength of the sheets to be processed and the particles applied to the surfaces of the partial sheets.
  • a plurality of partial sheets can be assembled into a thin and lightweight composite sheet.
  • the thickness reduction of the partial sheets and thus the resulting thickness of the composite sheet can be influenced by the pressure of the rolls.
  • the particles are sprayed onto the surface of at least one partial sheet.
  • Spraying is an easy-to-use and cost-effective coating process.
  • a spray gun it offers the possibility of rapid distribution of the particles on the surface.
  • the method allows a targeted grading of the particle distribution on a surface. A homogeneous distribution of the particles on the surface is of course also possible.
  • the particles are applied by means of a dipping process on the surface of at least one partial sheet.
  • This process also provides a simple and extremely cost-effective way of coating a surface.
  • the composite sheet may be dipped into the suspension or contacted with its surface and finally stored for drying.
  • a gradation of the particle layer can also be achieved. This is possible, for example, by immersing only certain areas of the partial sheet to be coated in a suspension or by controlled control of the peel-off. hens from the suspension.
  • the rate of removal also allows the amount deposited to be varied. With a slow removal of the sheet from the suspension, the particle layer is preferably thinner than with a rapid peel.
  • the thickness of the particle layer can be adjusted by a repeated successive immersion of the partial sheet, or the points to be coated.
  • the second object of the invention is achieved by a composite sheet with the feature combination according to claim 21.
  • the composite sheet is produced in particular by means of the aforementioned method and consists of a plurality of stacked, by roll cladding in each case interconnected partial sheets, between which homogeneously or selectively graded distributed particles, in particular nanoparticles are included.
  • the composite sheet consists of a plurality of partial sheets and can be widely used because of its increased strength and / or its functional properties and its low weight.
  • the controlled application of the particles during the passage of the ARB cycles allows the application of structured or graded coatings to a surface. In particular, by a gradient in the particle layer, the properties of the composite sheets can be influenced.
  • Such functionally graded materials are particularly well suited for lightweight construction.
  • a functionalization of the particle layers is possible, for example, by different electrical and / or thermal conductivity of the introduced in the individual layers of the composite sheet particles. These particles of different conductivities can either be applied together in one layer or in separate layers. The properties of the composite sheet are thus very specifically controllable.
  • a composite sheet with particles with an average diameter between 20 and 50 nm has a significantly increased strength over a composite sheet with larger or smaller particles.
  • the tensile strength of a composite sheet coated with Al 2 O 3 nanoparticles having a mean diameter of 25 nm was increased by about 13% over the pure roll-clad starting material.
  • such a composite sheet with a graded or even homogeneously distributed coating offers high load-bearing capacity and strength and, thanks to the simple and additionally flexible coating options, can be used for various fields of application.
  • the ARB process offers the possibility of producing such a composite sheet simply and inexpensively.
  • the suspension required for this was produced before the beginning of the coating of each partial sheet.
  • the particles were for the most part placed in a stirred ball mill and mixed with a solvent and, if appropriate, with a stabilizer. By grinding the particles in the stirred ball mill, a suspension with comminuted and finely divided particles could be obtained.
  • the suspensions were characterized before coating in terms of their properties in order to obtain conclusions about the particle sizes set by the grinding process and the stability of the suspension.
  • the particle size or particle diameter is the Sauter diameter.
  • the Sauter diameter describes the diameter of a monodisperse, spherical particle ensemble with the same specific surface area as the particle ensemble to be characterized.
  • Particle size was determined by DLS (Dynamic Light Scattering) and BET adsorption measurements.
  • SEM scanning electron microscope
  • BET adsorption measurements determine the specific surface area of the particles, from which the Sauter diameter can be deduced.
  • particle size distributions can be measured by means of light scattering. In this case, agglomerates are measured as such.
  • conclusions can be drawn on the dispersity of the particles.
  • Table 1 the values of the particle size distribution in terms of volume distribution are given as x y , 3, where y represents the percentage of measured particle agglomerates that is less than the specified value.
  • the values x 5 o, o represent the median of the number distribution.
  • Table 1 lists some values. The SEM images of various suspensions can be found in the description of the figures for FIG. 9.
  • partial sheets of aluminum AA1050A having a purity of 99.5% and a size of 300 mm ⁇ 100 mm ⁇ 1 mm were used.
  • the partial sheets were in cold rolled condition.
  • the aluminum part sheets were recrystallized at 500 ° C over a period of 1 hour. Finally, the partial sheets were quenched in water. The surface of the partial sheets was cleaned with acetone and finally roughened with a wire brush. This surface treatment removes soiling and eliminates unwanted surface oxides so that good adhesion of the particles to be applied in the next step and good cold welding can be ensured.
  • the suspension consisted of A 2 O 2 particles in water and was prepared in a stirred ball mill with a grinding time of 1 h.
  • Spherical grinding media of yttrium-stabilized zirconium dioxide having a diameter between 400 ⁇ m and 500 ⁇ m were used as grinding media.
  • an average torque of 2.05 Nm was achieved at an idling torque of 0.60 Nm.
  • the concentration of A ⁇ Oa particles in the suspension was 5% by weight, the average particle diameter was 10 nm.
  • nitric acid was used for electrostatic stabilization.
  • the pH of the suspension was 5.4.
  • the suspension or particles were applied to the surface by means of a dipping process. For this purpose, a container filled with the suspension was used, in which the partial sheets were brought with their surface in contact with the surface of the suspension. After removal of the partial sheet from the suspension tank, it was set up inclined to dry so that the excess solvent could drain off. This process was repeated every cycle.
  • the amount of particulate deposited on the surface during coating was about 0.1% by volume in total, based on the volume of the composite sheet, and the resulting particle layer had a thickness of about 0.6 ⁇ m, which is about 60 times the particle size.
  • the part laminations were each heat treated at 125 ° C. for 5 minutes to evaporate solvent still present on the surface and to exclude moisture from entering the interior of the sheet.
  • the heat treatment can increase the ductility of the composite sheet, resulting in improved bonding performance and increased bondline strength.
  • the resulting composite sheet with the particle layer trapped between the part sheets was then split and prepared again for roll cladding.
  • the part-plates arising during the division of the composite sheet are not recrystallized but their surface is directly cleaned and roughened.
  • the part sheets were then re-coated as described, stacked and joined by a rolling process including a particle coating. There were a total of 8 cycles. After completion of the process, ie after passing through the 8 cycles, the final composite sheet was finally subjected to curing. This curing took place over a period of 1 hour at a temperature of 150 ° C.
  • an increase in the hardness of the composite sheet by 8% compared to the uncured material could be achieved.
  • the resulting composite sheet has an increased tensile strength over the uncoated composite sheet. Due to the nearly constant density at a particle concentration of only 0.1% by volume, the increase in the specific strength of the composite sheet corresponds to the increase in tensile strength.
  • cold rolled aluminum sheet panels AA1050A having a purity of 99.5% and a size of 300 mm ⁇ 100 mm ⁇ 1 mm were used to produce the composite sheet.
  • the partial sheets were recrystallized for 1 hour at 500 ° C before the start of the process and finally also quenched in water.
  • the part panels were treated with acetone and roughened with a wire brush.
  • the suspension consisted of ZrO 2 particles with a particle diameter of 63 nm in water. This suspension was prepared by means of a stirred ball mill over a period of 5 hours, the concentration being 4.07% by weight. Spherical grinding media of yttrium-stabilized zirconium dioxide with a diameter between 400 ⁇ m and 500 ⁇ m were used as grinding media.
  • An average torque of 2.10 Nm was achieved with an idling torque of 0.60 Nm at a speed of the shaft with perforated disc stirrer with a diameter of 7 cm of 2200 min -1 , to prevent agglomeration of the particles as in Example 1 nitric acid used for electrostatic stabilization
  • the pH of the suspension can be given as 3.5.
  • the suspension or particles were applied to the surface by means of a spray process at a pressure of 4 bar. The spraying process was carried out uniformly during each of the 8 ARB cycles, with a total of 12 ml of the suspension being sprayed onto the surface.
  • the deposited particle volume was about 0.1% by volume of the final composite sheet.
  • the applied layer thickness in this embodiment is about 0.6 ⁇ in each of the 8 cycles, which corresponds to a particle size of 80 nm is about 7.5 times the particle size.
  • the resulting composite sheet with the particle layer trapped between the part sheets was then split and prepared again for roll cladding. Recrystallization was also carried out only before the first coating operation.
  • the partial sheets were coated again, stacked and connected by a rolling process including a particle coating. There were a total of 8 cycles.
  • the resulting composite sheet was subjected to curing for 1 hour at a temperature of 150 ° C to further increase hardness and tensile strength.
  • partial sheets of aluminum AA1050A having a purity of 99.5% and a size of 300 mm ⁇ 100 mm ⁇ 1 mm were used.
  • the partial sheets were in cold rolled condition.
  • the aluminum part sheets were also recrystallized at 500 ° C over a period of 1 hour, quenched in water and subjected to surface treatment with acetone and a wire brush. This surface treatment can remove soiling and eliminate unwanted surface oxides, so that good adhesion of the particles to be applied in the next step can be ensured.
  • the suspension consisted of SiC particles in water and was produced by means of autogenous comminution in the agitator ball mill PE 075 (Netzsch Feinmahltechnik GmbH) over a period of 24 hours.
  • the concentration of the SiC particles in the suspension was 5.14 wt .-% and the particles had a mean diameter of 26 nm.
  • grinding media was silicon carbide split "SiC dark FF 0.5-1 18/35" from ESK SiC GmbH with a diameter between 500 pm and 1000 pm
  • the speed of the stirrer was 1500 min -1 .
  • nitric acid was used as a stabilizer.
  • the pH of the suspension is 9.6. After completion of the comminution, the suspension was allowed to stand for 36 h. dimentiert and the deducted fraction of Mahl stresses separated. The separation of the suspension was achieved mainly by a pure settling let the Mahl Sciencesreste of the remaining suspension.
  • the suspension or particles were applied to the surface by means of a spray process at a pressure of 4 bar.
  • the spraying process was carried out 8 times in succession, with a total of 12 ml of the suspension being sprayed onto the surface.
  • the total deposited particle volume was after 8 cycles at 0.1 vol .-% of the finished composite sheet.
  • the thickness of the resulting particle layer was about. 0.6 pm, which is about 23 times the particle size with a mean diameter of 26 nm.
  • the particles can also be pressed into adjacent partial plates during the deformation under the roller, so that a layer thickness after rolling is mainly theoretically definable.
  • the part laminations were each heat treated at 125 ° C. for 5 minutes to evaporate solvent still present on the surface and to exclude moisture from entering the interior of the sheet.
  • the heat treatment can increase the ductility of the composite sheet, resulting in improved bonding performance and increased bondline strength.
  • the resulting composite sheet with the particle layer trapped between the part sheets was then split and re-plated for roll-plating prepared.
  • the partial sheets resulting from the division of the composite sheet were not recrystallized, but their surface was directly cleaned and roughened.
  • the part sheets were then re-coated as described, stacked and joined by a rolling process including a particle coating. There were a total of 8 cycles.
  • the composite sheet was finally subjected to curing.
  • the curing was carried out as in the previously described embodiments over a period of 1 hour at a temperature of 150 ° C.
  • composite sheets were made with titanium particles.
  • cold rolled aluminum partitions AA1050A with a purity of 99.5% and a size of 300 mm ⁇ 100 mm ⁇ 1 mm were used as in the previously described embodiments.
  • the aluminum part sheets were recrystallized over a period of 1 hour at 500 ° C and the surface freed by acetone and brushing of dirt.
  • the coating of the surface of the individual partial sheets was carried out from a suspension of titanium particles in water.
  • the particles in the suspension were unstabilized.
  • the aqueous suspension with a concentration of 21% by weight was prepared by means of "titanium metal powder E - in water” from Chemetall
  • the average size of the Blaine particles is between 2 ⁇ m and 4 ⁇ m.
  • the particles were applied by means of a spray method.
  • the spray pressure was 4 bar and the spraying process was only performed during cycles 1 to 6 of a total of 9 cycles. In each case, approximately 10 ml of the suspension were Pension sprayed on the surface.
  • the total particle fraction deposited was 5.4% by weight of the finished composite sheet.
  • the part sheets Prior to roll cladding, the part sheets were each heat treated at 125 ° C for 5 minutes to evaporate any solvent still present on the surface and to exclude moisture from entering the inside of the sheet. This heat treatment was performed in each of the nine cycles to increase the ductility of the composite sheet, resulting in improved bonding performance and increased bondline strength.
  • the resulting composite sheet was split and returned to the rolling process. Recrystallization was also performed only before the first rolling.
  • the part sheets were again coated, stacked and joined by a rolling process including a particle coating. A total of 9 cycles were run in which the composite sheets obtained from the previous cycle were each used as partial sheets for the next cycle.
  • the composite sheets produced in this way have an approximately 10% increased strength at almost the same density.
  • the specific strength as an important lightweight criterion is increased by almost 10%.
  • the finished composite sheet was heat treated after 6 cycles of particle introduction and 3 cycles without introduction of Ti particles for 1 hour to 8 days at temperatures between 350 ° C and 600 ° C.
  • the heat-treated sheets have a coarse-grained structure.
  • the Ti particles are completely converted to intermetallic phases after a maximum of 24 hours at 600 ° C. This represents a significant acceleration of the reaction compared to Ti-foil-reinforced aluminum sheets, which, depending on the size of the film fragments, take several days to weeks to convert completely to intermetallic phases.
  • the resulting intermetallic phases have a hardness of up to 10 GPa.
  • metal foam was produced from composite sheets produced. Partial aluminum sheets AA1050A with a purity of 99.5% and a size of 300 mm x 100 mm x 1 mm were used for this purpose. The partial sheets were in cold rolled condition.
  • the aluminum part sheets were recrystallized at 500 ° C over a period of 1 hour.
  • the surface was cleaned with acetone and roughened with a wire brush.
  • the coating of the surface of the individual partial sheets was carried out from a suspension of TiH 2 particles in water at a concentration of 33 wt .-%.
  • the suspension was prepared by means of "titanium hydride powder VM" from Chemetall.
  • the mean particle size Blaine is here 1, 6 pm to 2 ⁇ .
  • the suspension was unstabilized.
  • the particles were applied by means of a spray method.
  • the spray pressure was 4 bar and the spraying process was performed only during the first two of a total of 8 cycles. In each case, 7 ml of the suspension were sprayed onto the surface.
  • the total deposited particle volume was 0.4% by volume of the composite sheet.
  • the resulting particle layer after coating had a thickness of about 55 ⁇ , which corresponds approximately to 25 times an average particle size of 2 pm.
  • the coated composite sheet was heated above the melting point either by induction heating at a power between 1 and 2 kW for about 20-60 seconds or in the heat treatment furnace at temperatures between 700 and 1000 ° C for 1 to 15 minutes and then cooled in air. During heating, H 2 was released by thermal decomposition of the titanium hydride, the partially liquid aluminum foamed and a metal foam was formed from the composite sheet.
  • the foams produced in this way are characterized by a porosity of up to about 70%.
  • Another specific feature is the small thickness of foamable sheet and thus the foamed samples, which may represent an advantage over the prior art in certain applications.
  • the lead They can be rolled into thin foils in the range of 0.1-0.5 mm thickness and then foamed.
  • composite sheets were made with copper particles.
  • 16 cold-rolled aluminum partitions AA1050A with a purity of 99.5% and a size of 37.5 mm x 100 mm x 1 mm were used.
  • the aluminum part sheets were recrystallized over a period of 1 hour at 500 ° C and the surface freed by acetone and brushing of dirt.
  • the coating of the surface of the individual partial sheets was carried out from a suspension of copper particles in water.
  • the particles in the suspension were unstabilized.
  • the aqueous suspension with a concentration of 33% by weight was prepared by means of "copper powder MicroTronic 120" from Ecka Granules
  • the average size of the particles, determined by laser diffraction, is between 1.5 ⁇ m and 2.5 ⁇ m.
  • the particles were applied by means of a spray method.
  • the spray pressure was 4 bar and the spraying process was carried out in each of the 4 total cycles.
  • the partial plates were coated in each cycle over its length with varying the relative velocity of the spray gun and the sheet in a range of 0.1 m / s and 1, 0 m / s and with simultaneous variation of the spray distance between 15 cm and 28 cm. This creates a continuous gradient in the amount of copper deposited over the length of the sheet.
  • the part-plates were each heat-treated at 125 ° C. for 5 minutes to evaporate the solvent still present on the surface and to prevent moisture from being trapped inside the sheet. This heat treatment was performed in each of the nine cycles to increase the ductility of the composite sheet, resulting in improved bonding performance and increased bondline strength.
  • the graded composite sheet thus produced also has graded mechanical and functional properties as a function of position in the sheet length direction.
  • the strength of the material is increased by up to 10% compared to an identical sheet without copper particles.
  • the increase in strength varies over the length of the sheet with the copper content.
  • the electrical conductivity of the graded composite sheet is increased compared to an identical sheet without copper particles.
  • the increase in conductivity varies over the sheet length between 0 and 15%.
  • the graded composite sheet shows increased specific strength and increased conductivity over a non-particle reinforced identical sheet.
  • the expression of the property improvement is a function of the position in the sheet length and thus the copper content.
  • the copper was dissolved in the aluminum during a heat treatment at 530 ° C for 48 hours. This recrystallizes the aluminum and the copper particles are dissolved in the aluminum matrix.
  • the result is a composite sheet of aluminum with continuously graded varying dissolved copper content and thus different binary Al-Cu alloys as a function of the sheet length. These can be detected by examining the strength over the greatly different solid solution hardening effect.
  • the strengths in the sheet vary between 80 and 180 MPa.
  • the sheet After the recrystallization annealing, the sheet can be returned to the cyclic rolling process as described above without particle introduction. As a result, the ultrafine-grained structure in the composite sheet with dissolved copper can be restored. As a result, high strength can be achieved in the commercial Al-Cu alloys of the AA2xxx series, for example about 400 MPa after three cycles.
  • the abovementioned process has the advantage of producing locally different compositions via the graded particle reinforcement.
  • Embodiment 7 Furthermore, there is the possibility of a targeted heat treatment for precipitation hardening in the recrystallized state or after repeated rolling.
  • composite sheets were made of a technical Al alloy with copper particles.
  • cold-rolled aluminum partitions AA2017A and with a size of 300 mm x 100 mm x 1 mm were used.
  • the aluminum part sheets were solution-annealed at 530 ° C for a period of 30 minutes and the surface was cleaned of contaminants by acetone and brushing.
  • the coating of the surface of the individual partial sheets was carried out from a suspension of copper particles in water.
  • the particles in the suspension were unstabilized.
  • the aqueous suspension with a concentration of 33% by weight was prepared by means of "copper powder MicroTronic 120" from Ecka Granules
  • the mean particle size, determined by laser diffraction, is between 1.5 ⁇ m and 2.5 ⁇ m.
  • the particles were applied by means of a spray method.
  • the spray pressure was 4 bar and the spraying process was carried out in each of the 3 total cycles.
  • the total deposited particle volume was after 3 cycles at 0.1 vol .-% of the finished composite sheet.
  • the part laminations were each heat-treated at 125 ° C. for 5 minutes to evaporate the solvent still present on the surface and to exclude moisture from entering the interior of the sheet.
  • the heat treatment can increase the ductility of the composite sheet, resulting in improved bonding performance and increased bondline strength.
  • the resulting composite sheet with the particle layer trapped between the part sheets was then split and prepared again for roll cladding.
  • the partial sheets resulting from the division of the composite sheet were not recrystallized, but their surface was directly cleaned and roughened.
  • the part sheets were then re-coated as described, stacked and joined by a rolling process including a particle coating. A total of 3 cycles were run through and achieved a particle content of about 0.2 vol .-%.
  • the strength of the material thus produced could be increased from 490 MPa of the same material after identical process control without particle application to about 560 MPa. This represents an improvement of about 15%. Again, this increase in strength has been achieved with almost no density change, which has increased the specific strength by almost the same amount.
  • composite sheets of high-purity oxide-free copper OF-Cu99.99 were used.
  • recrystallized partial sheets of copper OF-Cu99.99 with a size of 300 mm ⁇ 100 mm ⁇ 1 mm were used.
  • the surface was cleaned by acetone and brushing of dirt.
  • the coating of the surface of the individual partial sheets was carried out from a suspension of aluminum particles in water.
  • the particles were in the suspension unstabilized.
  • the aqueous suspension with a concentration of 33% by weight was prepared by means of "Ecka Aluminum Grit AS ⁇ 10 ⁇ m MEP105 RE0902" from Ecka Granules
  • the mean size of the particles, determined by Fisher, is 5 ⁇ m.
  • the particles were applied by means of a spray method.
  • the spray pressure was 4 bar and the spraying process was only performed during cycles 1 to 6 of a total of 9 cycles.
  • the total particle fraction deposited was 1.0% by weight of the finished composite sheet.
  • the part sheets were each heat-treated at 125 ° C. for 5 minutes to evaporate the solvent still present on the surface and to prevent moisture from being trapped inside the sheet.
  • the heat treatment can increase the ductility of the composite sheet, resulting in improved bonding performance and increased bondline strength.
  • the composite sheets produced by means of the method have different mechanical and / or functional properties, in particular depending on the process and coating parameters. Accordingly, experiments are given in addition to the aforementioned embodiments in the following. This shows: 1 the influence of the suspension medium and the rolling temperature on the tensile strength and on the extensibility of an uncoated composite sheet,
  • Fig. 7 shows the influence of the curing temperature on the hardness of a finalized
  • Fig. 8 shows the influence of the number of the processed process cycles on the
  • Fig. 9 photographs of a scanning electron microscope (SEM images) for determining the stability and morphology of various suspensions.
  • SEM images scanning electron microscope
  • the values shown in the figures are mean values.
  • the experiments were carried out with composite sheets from different production batches (batch 1 and batch 2).
  • the values are accordingly to be understood in relation to the reference lines indicated in the respective plots.
  • Fig. 1 shows the influence of the suspension medium and the rolling temperature on the tensile strength and extensibility of an uncoated composite sheet in a plot of tensile strength [MPa] versus extensibility [%].
  • MPa tensile strength
  • % extensibility
  • the values that could be determined for a rolling operation at 125 ° C show that at this temperature, the liquid medium has no significant impact on tensile strength and ductility of the composite sheet.
  • the tensile strength therefore has approximately the same value regardless of whether ethanol (15b), water (15c) or no liquid (15a) is applied.
  • a clear increase in tensile strength is recorded, but also independent of the medium, ie ethanol (17a) or water (17b). This is due to the increased bond strength at elevated rolling temperature.
  • FIG. 2 shows a plot 21 of the tensile strength [MPa] versus the particle diameter [nm].
  • both the values 23 obtained after the coating by means of a spraying method and the values 25 determined by a dipping method are approximately the same.
  • the tensile strength of a coated composite sheet has therefore been increased with both coating methods. Furthermore, no significant change in the tensile strength with increasing particle size can be determined in the context of the specified error tolerances in both methods. Compared to the reference 27, ie the uncoated part sheet, an equal increase of the tensile strength is achieved by both methods.
  • FIG. 3 shows a further plot 31 of the tensile strength [MPa] against the particle diameter [nm] of Al 2 O 3.
  • the influence of the layer thickness of the applied particles on the tensile strength of a composite sheet shown as a function of the particle diameter.
  • the particle diameter was varied between 7 nm and 170 nm.
  • Three series of composite sheets 33, 35, 37 were investigated, which were each coated with A ⁇ Oa particles from an aqueous suspension. Coating was performed once for composite sheets 33 of the first series, three times for composite sheets 35 of the second series and six consecutive times in composite sheets 37 of the third series.
  • the composite sheets 33 of the first series after the simple spraying and the resulting thin coating the highest tensile strength compared to the other composite sheets 35, 37 of the second and third series of experiments.
  • the values for the multi-coated composite sheets 35, 37 are below the values of the reference measurement 39, in particular for small particle sizes. This is due to the decreasing bond strength due to the decreasing metal-metal contact with increasing layer thickness between the partial sheets.
  • the associated values can be found in the following Table 3.
  • 170 3 x spraying 179.8 ⁇ 2.0 4 shows a plot 41 of the tensile strength [MPa] against the particle diameter [nm] for determining the influence of the suspension medium and the stabilizer on the tensile strength of a coated composite sheet as a function of the particle diameter.
  • Four different series of composite sheets 43, 45, 47, 49 were investigated, each coated with Al2O3 particles. Both the solvent (water and ethanol) and the stabilizer (nitric acid and propionic acid) were varied. In addition, the temperature of the rolling process was varied between 20 ° C and 125 ° C.
  • the lines 43a, 45a and 47a respectively denote the reference measurements for the uncoated sheets.
  • the series of composite sheets 43 has been coated with Al 2 O 3 particles of aqueous and nitric acid stabilized suspension and rolled at 125 ° C.
  • the three remaining series of composite sheets 45, 47, 49 have been coated with Al 2 O 3 particles from a suspension with ethanol.
  • the composite sheet coating suspension 45 was stabilized with nitric acid, and the coated composite sheets 45 were each rolled at 125 ° C. However, the resulting tensile strength values of the series of composite sheets 45 are significantly below the values for the composite sheets 43. Also, the tensile strength is less than that of the reference measurement 45a.
  • the series of composite sheets 49 has also been rolled in accordance with the composite sheets 43 and 45 at 125 ° C. Unlike all other samples, the suspension was stabilized with propionic acid for coating rather than nitric acid. The tensile strength is increased over the composite sheets 45, although the only difference in the production of the composite sheet series 49 was in the use of another stabilizer. The resulting Difference in tensile strength values of the composite sheets 45, 49 can be explained by different surface states of the particles with respect to electrostatic stabilization and surface chemistry.
  • Fig. 5 shows a plot 51 of tensile strength [MPa] versus particle diameter [nm], which reflects the influence of particulate material and particle size on the tensile strength of a composite sheet.
  • four series of composite sheets 53, 55, 57, 59 are coated with different particles from an aqueous suspension. The particle diameter was varied between 7 nm and 170 nm.
  • the first series of composite sheets 53 was coated with A Oa particles.
  • the second and third series of composite sheets 55, 57 were coated with ⁇ 1 ⁇ 2 and SnO2 particles, respectively.
  • the coating of the fourth composite sheet series 59 was carried out with SiC particles.
  • the composite sheets 53 coated with Al 2 O 3 particles have the highest tensile strength in relation to the reference line 53 a. This then steadily decreases, from the composite sheets 53 coated with Al 2 O 3 particles over SiC, ZrO 2, up to the series of composite sheets 57 coated with SnO 2 particles. The trend also shows for all series of different composite sheets 53, 55, 57, 59, regardless of the type of particles used for the coating, an increase in the tensile strength at average particle diameters and a subsequent decrease with increasing particles.
  • FIG. 6 shows a plot 61 of the strain rate dependence of a composite sheet as a function of the particle diameter [nm] for composite-coated composite sheets.
  • the strain rates used for comparison were 10 "3 s " 1 and 10 "5 s " 1 .
  • the particle diameter has no appreciable influence on the strain rate dependence of the composite sheet series 63, 65, 67, 69. Only the values of a recrystallized sheet 70 shown for comparison differ. Furthermore, the strain rate dependence is also largely independent of the nature of the particles used. The values determined are all of the order of magnitude of the reference line, regardless of the particle size or the particle diameter and their type. For reasons of clarity, only one associated data point is marked in FIG. A tabular listing of all data shown is shown in Table 4.
  • Fig. 7 shows plot Vickers hardness HV5 versus cure temperature [° C] for A ⁇ Oa particle coated composite sheets.
  • the particle diameters were varied between 10 nm and 170 nm.
  • the re- resulting values are plotted relative to reference 73a.
  • the composite sheets 73, 75, 77, 79 were cured for one hour.
  • the temperature was varied between 125 ° C and 350 ° C for this purpose.
  • the subsequent Vickers hardness test was carried out with an indentation force of 49.05 N and a holding time of 10 s at four different points of the sheet.
  • the curves of the values for the individual composite sheets 73, 75, 77, 79 clearly show the influence of the curing temperature on the hardness of each finalized composite sheet as a function of the particle diameter. It can be seen that the hardness of all samples after a one-hour heat treatment at 150 ° C compared to the samples stored at room temperature is increased and finally decreases continuously. The trend here is similar regardless of the particle size. However, it can be seen that the increase after a heat treatment at 150 ° C for the composite sheets, which are reinforced with nanoparticles with an average diameter between 10 nm and 25 nm, is significantly higher than with the larger particles and the unreinforced reference. The associated values are shown in Table 5.
  • Table 5 Dependence of the Vickers hardness HV5 of the coated composite sheets of different hardening temperatures [° C] and for AI2O3 particles with different particle diameters [nm] after a curing time of 1 hour.
  • Figure 8 shows a plot 81 of tensile strength versus number of ARB cycles swept.
  • the examined composite sheet 83 is coated with Al 2 O 3 particles with a diameter of 10 nm.
  • a measurement point 85 is shown after 8 cycles.
  • FIG. 9 shows photographs 91 of a scanning electron microscope of various suspensions after the respective grinding time.
  • Figs. 9 (a) to (c) show Al 2 O 3 particles in water before grinding (a), after one hour (b) and after 24 hours (c).
  • the distribution of the particles in the suspension changes with time from coarse-grained particles before grinding to finer but partially agglomerated particles to very fine particles evenly distributed with a comparable diameter.
  • Fig. 9 (d) shows a partially agglomerated suspension with Al 2 O 3 particles in ethanol after one hour and is thus comparable to Fig. 9 (b).
  • Fig. 9 (e) shows a suspension of Z particles finely dispersed in water after 5 hours, whereas the suspension of Fig. 9 (f) shows an agglomeration of SnO 2 after 43 hours in water.
  • most manufactured suspensions are Al 2 O 3 particles in both water and in ethanol stable to agglomeration, whereas the suspensions of Zr0 2 particles and especially Sn0 2 particles used tend to agglomerate.

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Abstract

L'invention concerne un procédé de fabrication d'une tôle composite métallique multicouches, comprenant les étapes de procédé suivantes : enduction d'une surface d'une première tôle partielle par application de particules, empilement de la première tôle partielle avec la surface recouverte sur une surface d'une seconde tôle partielle, liaison des tôles partielles par plaquage par laminage avec inclusion des particules appliquées pour former une première tôle composite, et éventuellement répétition des étapes susmentionnées avec l'utilisation de la première tôle composite comme tôle partielle pour la formation d'une tôle composite à partir d'une pluralité de tôles partielles. Dans le cas présent, il est prévu d'appliquer les particules provenant d'une suspension sur la surface d'une zone partielle ou de chaque zone partielle. Un tel procédé permet la fabrication simple d'une tôle composite ayant des propriétés mécaniques et/ou fonctionnelles, améliorées de façon ciblée, ou des propriétés de matériau graduées de façon ciblée. L'invention concerne également une tôle composite qui est fabriquée avec le procédé susmentionné.
EP11727639A 2010-05-15 2011-05-12 Procédé de fabrication d'une tôle composite métallique multicouche en utilisant une suspension de particules; tôle composite correspondante Withdrawn EP2571653A1 (fr)

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