EP2526216A1 - Method for manufacturing 6xxx alloy materials for vacuum chambers - Google Patents

Method for manufacturing 6xxx alloy materials for vacuum chambers

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Publication number
EP2526216A1
EP2526216A1 EP11706295A EP11706295A EP2526216A1 EP 2526216 A1 EP2526216 A1 EP 2526216A1 EP 11706295 A EP11706295 A EP 11706295A EP 11706295 A EP11706295 A EP 11706295A EP 2526216 A1 EP2526216 A1 EP 2526216A1
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EP
European Patent Office
Prior art keywords
weight
block
thickness
temperature
optionally
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.)
Granted
Application number
EP11706295A
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German (de)
French (fr)
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EP2526216B1 (en
Inventor
Cédric GASQUERES
Joost Vankappel
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Constellium Valais AG
Constellium Issoire SAS
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Constellium Valais AG
Constellium France SAS
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Publication of EP2526216A1 publication Critical patent/EP2526216A1/en
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/02—Alloys based on aluminium with silicon as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
    • C22C21/08—Alloys based on aluminium with magnesium as the next major constituent with silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • C22F1/05—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys of the Al-Si-Mg type, i.e. containing silicon and magnesium in approximately equal proportions

Definitions

  • the invention relates to the manufacture of 6xxx alloy products, in particular intended to be used in the production of vacuum chambers for the manufacture of integrated electronic circuits based on semiconductors, flat display screens and photovoltaic panels. .
  • the blocks must first have satisfactory mechanical characteristics to achieve by machining parts having the desired dimensions and rigidity so as to reach, without deformation, a vacuum generally at least the level of the average vacuum (10 " - 10 " Torr).
  • the desired breaking strength (R m ) is generally at least 260 MPa and even more preferably if possible.
  • the residual stresses in the blocks intended to be machined in the mass must be low so as to reach the desired dimensions without difficulty and without deformation during machining. Since the dimensions of the vacuum chambers increase continuously, especially for the production of liquid crystal panels or large photovoltaic panels, it is necessary to produce increasingly thick aluminum alloy blocks, particularly from minus 250 mm or even 300 mm thick. The thicker the blocks, the more difficult it is to obtain sufficient mechanical properties while maintaining excellent machining stability.
  • the level of porosity of the blocks must also be low enough to reach the high-vacuum (10 6 - 10 "8 Torr) if necessary, and the gases used in the vacuum chambers are frequently very reactive and so as to avoid the risks of pollution of silicon wafers or liquid crystal devices by particles or substances from the walls of vacuum chambers and / or frequent replacement of parts, it is important to protect the surfaces of the rooms.
  • 'proves to be a material advantageous from this point of view because it is generally possible to perform anodizing a hard oxide layer on the surface of the blocks, resistant to reactive gases.
  • the strength of the anodic layer is affected by many factors related in particular to the microstructure of the product (grain size, phase precipitation, porosity) and it is always desirable to improve this parameter.
  • U.S. Patent No. 6,565,984 discloses an alloy suitable for the manufacture of semiconductor manufacturing chambers of composition (in% by weight) Si: 0.54 - 0.74; Cu: 0.15-0.30; Fe: 0; 05 - 0; 20; Mn ⁇ 0.14; Zn ⁇ 0.15; Cr: 0.16 - 0.28; Ti ⁇ 0.06; Mg: 0.9-1.1.
  • the pieces are obtained by extrusion or machining to the desired shape.
  • the composition makes it possible to control the size of the impurity particles, which improves the performance of the anodic layer.
  • No. 6,982,121 Koreanyu Mitsui Aluminum discloses an alloy suitable for anodizing and adapted to plasma treatment chambers containing (in% by weight) Mg: 2.0 to 3.5; Ti: 0.004 to 0.01% and the remaining aluminum of purity 99.9%.
  • the alloy does not require heat treatment, unlike alloys requiring the precipitation of Mg 2 Si.
  • the alloy does not require the presence of Cr and Mn which must be added to alloys 5052 and 6061 to control the size of the alloy. grain, but which may cause pollution of heavy metals treated semiconductors.
  • the mechanical characteristics of the alloy are however not indicated.
  • the cost of 99.9% pure aluminum is high.
  • US Patent Application 2009/0050485 discloses a composition alloy (in% by weight) Mg: 0.1 - 2.0; If: 0.1 - 2.0; Mn: 0.1 - 2.0; Fe, Cr, and Cu ⁇ 0.03, anodized so that the hardness of the anodic oxide layer varies in thickness.
  • the very low content of iron, chromium and copper leads to a significant additional cost for the metal used.
  • the patent application EP 2 003 219 A2 (Kobe Steel) describes a forging alloy comprising (in% by weight) Mg 0.5 - 1.25%, Si: 0.4 - 1.4%, Cu: 0, 01 - 0.7%, Fe: 0.05 - 0.4%, Mn: 0.001 - 1.0%, Cr 0.01 - 0.35%, Ti and Zr 0.005 - 0.1%.
  • this document discloses products obtained by performing a hot forging step prior to dissolution.
  • a first object of the invention is a method of manufacturing an aluminum block with a thickness of at least 250 mm intended for the production of elements for vacuum chambers in which, successively,
  • composition alloy block in% by weight, Si: 0.5 - 1.5; Mg: 0.5-1.5; Fe ⁇ 0.3; Cu ⁇ 0.2; Mn ⁇ 0.8; Cr ⁇ 0.10; Ti ⁇ 0.15; other elements ⁇ 0.05 each and ⁇ 0.15 in total, remaining aluminum;
  • the cast block is homogenized at a temperature between 500 ° C and 590 ° C;
  • a solution heat treatment is carried out at a temperature of between 450 ° C. and 560 ° C. directly on the cast block and optionally homogenized, without producing a hot or cold deformation step solution beforehand;
  • Another subject of the invention is a block of composition, in% by weight, Si: 0.5 - 1.5; Mg: 0.5-1.5; Fe ⁇ 0.3; Cu ⁇ 0.2; Mn ⁇ 0.8; Cr ⁇ 0.10; Ti ⁇ 0.15 other elements ⁇ 0.05 each and ⁇ 0.15 in total, remains aluminum, with a thickness of at least 250 mm, and having, in the T6 or T652 state, a breaking strength R m at 1 ⁇ 4 thickness at least equal to 280 MPa and an elastic limit R p o, 2 to 1 ⁇ 4 thickness at least equal to 240 MPa, obtained by semi-continuous casting, optionally homogenization of the cast block at a temperature between 500 ° C and 590 ° C., dissolved at a temperature of between 450 ° C.
  • Yet another object of the invention is the use of a block according to the invention in the production of vacuum chambers for the manufacture of integrated electronic circuits based on semiconductors, flat display screens and / or or that of photovoltaic panels.
  • FIG 1 Granular structure of the blocks obtained by the process according to the invention 11 (FIGla) and 21 (FIGlb).
  • FIG. 2 Granular structure of the reference block 31 (FIG. 2a) and of the block obtained by a method according to the prior art (deformation by fofage before dissolution) (FIG. 2b). Detailed description of the invention
  • the designation of the alloys is in accordance with the regulations of The Aluminum Association (AA), known to those skilled in the art.
  • the definitions of the metallurgical states are given in the European standard EN 515.
  • the static mechanical characteristics in other words the ultimate tensile strength Rm, the conventional yield stress at 0.2% elongation Rp0.2 and the elongation at break A%, are determined by a tensile test according to EN 10002-1, the sampling and the direction of the test being defined by EN 485-1. Hardness is measured according to EN ISO 6506.
  • the elements for vacuum chamber include vacuum chamber bodies, valve bodies, flanges, connecting elements, sealing elements, passages, flexible pipes.
  • an alloy of the 6xxx family is converted into a block that can be used for the production of elements for vacuum chambers without producing a hot or cold deformation step solution before being put into solution.
  • a block of thickness at least equal to 250 mm of alloy composition (in% by weight) Si: 0.5 - 1.5; Mg: 0.5-1.5; Fe ⁇ 0.3; Cu ⁇ 0.2; Mn ⁇ 0.8; Cr ⁇ 0.10; Ti ⁇ 0.15; other elements ⁇ 0.05 each and ⁇ 0.15 in total, aluminum remains is obtained by semi-continuous casting, optionally homogenization of the cast block at a temperature between 500 ° C and 590 ° C; dissolving at a temperature of between 450 and 560 ° C.
  • the iron content must be less than 0.3% by weight because beyond this value, the anodic layer obtained to protect the metal from the reactive gases does not reach the desired resistance.
  • the present inventors have found, however, that it is not necessary to achieve a very high level of purity to obtain anodic layers having the desired characteristics with the process according to the invention.
  • the iron content is advantageously at least 0.1% by weight, which makes the process according to the invention particularly economical.
  • the copper content must be less than 0.2% by weight because a too high copper content increases the quenching sensitivity. It is however advantageous in some cases to add a limited amount of copper to improve the mechanical characteristics, especially when the cooling rate after dissolution is greater than 800 ° C / h.
  • a copper content of between 0.03 and 0.15% by weight is preferred in one embodiment of the invention. The present inventors have found that if the chromium content is not less than 0.10% by weight, the desired mechanical properties, in particular the minimum mechanical strength, are not achieved. It is commonly accepted that for the realization of a wrought product for the 6xxx family vacuum chamber the presence of chromium and / or manganese is necessary in order to control the grain size.
  • the present inventors have found that in the context of the present invention, the absence of chromium is on the contrary favorable because without degrading the granular structure it makes it possible to limit the sensitivity to quenching and to improve the mechanical characteristics of the thick products.
  • the chromium content is less than 0.05% by weight and preferably less than 0.03% by weight.
  • the manganese content must in turn be less than 0.8% by weight, a content greater than 0.8% by weight being detrimental especially with regard to the properties of the anodic layer and the contamination of the vacuum chamber.
  • the manganese content is less than 0.6% by weight to prevent the formation of coarse phases which may be harmful for the properties of the anodic layer.
  • the manganese content is even less than 0.05% by weight.
  • the present inventors have found that, surprisingly, even in the absence of Cr, Mn and Zr, the granular structure obtained by the process according to the invention is controlled and makes it possible to obtain satisfactory characteristics in terms of mechanical properties and resistance to reactive gases.
  • the simultaneous absence of Cr, Mn and Zr thus makes it possible to very significantly reduce the sensitivity to quenching of the alloy and thus to improve the mechanical properties of the thick products, without degrading the granular characteristics and the properties of the anodic layers.
  • the contents of Cr, Mn and Zr are simultaneously less than 0.05% by weight and preferably less than 0.03% by weight.
  • the silicon and magnesium contents are between 0.5 and 1.5% by weight.
  • the combination of 0.5 to 0.8% by weight of silicon with 0.8 to 1.2% by weight of magnesium or the combination of 0.8 to 1.2% is produced. by weight of silicon with 0.6 to 1.0% by weight of magnesium.
  • the silicon content is between 0.8 and 1% by weight and preferably between 0.85 and 0.95% by weight and the content magnesium is between 0.6 and 0.8% by weight and preferably between 0.65 and 0.75% by weight.
  • the casting of the alloy is carried out by semi-continuous casting with direct cooling in block form. Typically, a block format having a thickness between 300 and 450 mm is used.
  • the cast block may optionally be homogenized at a temperature between 500 ° C and 590 ° C for at least one hour. Achieving homogenization is advantageous because it generally makes it possible to achieve more advantageous mechanical properties and better properties of the anodic layer and also to reduce the dissolution time.
  • the homogenization can be carried out during a separate heat treatment or alternatively during the solution heat treatment.
  • a surface machining also called “scalping" of the order of at least 5 mm per face, so as to eliminate the segregated layer on the surface and avoid the presence of cracks.
  • a solution heat treatment is then carried out directly on the cast block and optionally homogenized at a temperature of between 450 and 560 ° C., and preferably between 520 and 550 ° C. directly without a prior hot or cold deformation step.
  • Hot deformations conventionally of the processes of the prior art are generally carried out by rolling and / or forging and / or spinning.
  • the block does not undergo between the casting and the setting solution of significant deformation step by wrought.
  • Spinning is typically understood to mean rolling and / or forging and / or spinning operations.
  • none of the dimensions of the cast block undergo significant modification, that is to say typically at least about 10% by wrought between the casting and the implementation. solution.
  • the dissolution time is preferably greater than one hour.
  • the method according to the invention which avoids hot or cold deformation before dissolution is particularly advantageous from an economic point of view because this step is expensive. According to the prior art, this type of process was not envisaged especially for blocks intended for the realization of elements for 6xxx alloy vacuum chambers, probably because it was feared that, without heat deformation, the mechanical characteristics, the resistance of the anode layers and the level of porosity necessary to make elements for vacuum chamber are not achieved. In addition, some particularly thick products were not accessible by the methods according to the prior art. Surprisingly, the present inventors have found that the method thus simplified not only makes it possible to achieve properties equivalent to those obtained by the method according to the prior art, but in certain cases to exceed them.
  • the quenching step is critical, and must be performed with a cooling rate between the solution temperature and 200 ° C at least equal to 200 ° C / h.
  • the cooling rate is calculated at the mid-thickness of the blocks. If the cooling rate is too low, the present inventors have found that the desired mechanical properties are not achieved.
  • the cooling rate is between 200 ° C / h and 400 ° C / h.
  • the cooling rate is between 200 ° C./h and 400 ° C./h.
  • Such a cooling rate can be obtained by means of mist spray.
  • the cooling rate is at least 800 ° C./h.
  • a cooling rate can be obtained by spraying or immersion in water. Since a cooling rate that is too high can generate excessive internal stresses in the blocks, it is preferable to use water at a temperature of at least 50 ° C. for cooling.
  • the block thus hardened is stripped, preferably by cold compression with a permanent deformation rate of between 1% and 5%.
  • stress relief is particularly advantageous. The stress relieving allows to reduce the residual stresses in the metal and to avoid the deformations during the machining.
  • the tempering temperature is preferably between 150 and 190 ° C and preferably between 165 and 185 ° C, the duration of income being between 5 and 40 hours and preferably between 8 and 20 hours.
  • an income is obtained to reach the T6 or T652 state, corresponding to the peak of the static mechanical properties (R m and R p o, 2 ).
  • the blocks obtained by the process according to the invention are characterized by high mechanical properties.
  • the tensile strength R m at 1 ⁇ 4 thickness of the products obtained by the process according to the invention is at least equal to 280 MPa and the yield strength R p o, 2 at 1 ⁇ 4 thickness is at least equal to 240 MPa at 1 T6 or T652 state.
  • an alloy of composition Si 0.5 - 1.2; Mg 0.6-1.0; Fe 0, 1 - 0.3; Cu ⁇ 0.2; Mn ⁇ 0.05; Cr ⁇ 0.05; Ti ⁇ 0.15; other elements ⁇ 0.05 each and ⁇ 0.15 in total, and in the T6 or T652 state a breaking strength R m is obtained at 1 ⁇ 4 thickness of at least 300 MPa and an elastic limit R p o, 2 to 1 ⁇ 4 thickness is at least equal to 270 MPa, and more if the silicon content is between 0.8 and 1% by weight and preferably between 0.85 and 0.95% by weight and the magnesium content is between 0.6 and 0.8% by weight and preferably between 0.65 and 0.75% by weight, a rupture strength R m at 1 ⁇ 4 thickness at less than 320 MPa and a yield strength R p0.2 at 1 ⁇ 4 thickness is at least equal to 300 MPa in the T6 or T652 state.
  • a minimum value of elongation of at least 0.5% is reached by the products according to the invention in the T6 or T652 state. In some cases a minimum elongation value of at least 4% is reached by the products according to the invention.
  • the granular structure of the products according to the invention is characteristic of the absence of wrought before dissolution. Thus it is possible to distinguish the products according to the invention of the products according to the prior art for which hot or cold deformation is performed before the dissolution in solution by a simple metallographic examination.
  • the granular structure of the products according to the invention is isotropic, with an average grain size of at least 200 ⁇ .
  • the blocks obtained by the process according to the invention are suitable for use in the production of vacuum chambers for the manufacture of integrated electronic circuits based on semiconductors, flat display screens and / or photovoltaic panels.
  • the machining behavior of the blocks is favorable, thanks in particular to the high mechanical characteristics and the low level of residual stresses.
  • the anode layers obtained on the blocks machined by the usual anodizing processes are resistant to the reactive gases used in the vacuum chambers.
  • the blocks obtained by the process according to the invention can also be advantageously used for any other application in which the properties obtained are favorable.
  • Example in this example the process according to the invention was compared with a method according to reference examples.
  • the process according to the invention has been applied to two different alloys.
  • Four alloy blocks, the composition of which is given in Table 1, were cast by direct-cooling semi-continuous casting.
  • the blocks were scalped to a thickness of 410 mm. Table 1.
  • Composition of the alloys tested (% by weight)
  • the blocks were homogenized at a temperature between 540 and 590 ° C for a period of at least 4 hours.
  • 540 ° C and 200 ° C was about 1500 ° C / h), while the block 12 was quenched with air the average cooling rate between 540 ° C and 200 ° C was about 90 ° C / h.
  • the different blocks then underwent a cold compression of 1.5 to 2.5% and then experienced an income at 165 ° C so as to obtain a T652 state.
  • Table 2 Mechanical characteristics obtained (T652 state) after sampling at 1 ⁇ 4 thickness in the TL direction.
  • the blocks obtained by the process according to the invention (11 and 21), have a higher mechanical strength (Rm, Rp0,2) than that obtained with the reference ingots, the mechanical strength obtained with the ingot 11 being particularly advantageous.
  • the blocks obtained according to the invention had low residual stresses which avoids the deformation of the blocks during machining.
  • the level of porosity observed in the blocks according to the invention was very low, sufficiently low to reach high-vacuum.

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  • Organic Chemistry (AREA)
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Abstract

The invention relates to a method for manufacturing an aluminum block having a thickness at least equal to 250 mm and intended for manufacturing elements for vacuum chambers. Said method involves the following consecutive steps: semi-continuous casting of an alloy block having a composition such that, in wt%, Si is between 0.5 and 1.5, Mg is between 0.5 and 1.5, Fe < 0.3, Cu < 0.2, Mn < 0.8, Cr < 0.10, Ti < 0.15, each other element is less than 0.05, and a total of 0.15 remains aluminum; solution heat treatment is carried out, at a temperature between 450° and 560° C, directly on the cast block that is possibly made uniform; the resulting solution heat-treated block is quenched with the speed for cooling, between the solution temperature and 200° C, being at least 200° C/h; and tempering is carried out on the thus-quenched and possibly de-tensioned block. The resulting blocks are particularly advantageous in creating vacuum chambers for the manufacture of semiconductor-based integrated electronic circuits, flat display screens, and photovoltaic panels.

Description

Procédé de fabrication de produits en alliage 6xxx pour chambres à vide  Process for manufacturing 6xxx alloy products for vacuum chambers
Domaine de l'invention Field of the invention
L'invention concerne la fabrication de produits en alliage 6xxx, notamment destinés à être utilisés dans la réalisation de chambres à vide pour la fabrication de circuits électroniques intégrés à base de semi-conducteurs, d'écrans d'affichage plats ainsi que de panneaux photovoltaïques. The invention relates to the manufacture of 6xxx alloy products, in particular intended to be used in the production of vacuum chambers for the manufacture of integrated electronic circuits based on semiconductors, flat display screens and photovoltaic panels. .
Etat de la technique State of the art
Dans la fabrication des blocs en alliage d'aluminium destinés à être utilisés dans la réalisation de chambres à vide pour la fabrication de circuits électroniques intégrés à base de semi-conducteurs, d'écrans d'affichage plats ainsi que de panneaux photovoltaïques, il est important d'atteindre un ensemble de propriétés, tout en limitant le coût des opérations. In the manufacture of aluminum alloy blocks intended to be used in the production of vacuum chambers for the manufacture of integrated electronic circuits based on semiconductors, flat display screens as well as photovoltaic panels, it is important to achieve a set of properties, while limiting the cost of operations.
En effet, les blocs doivent tout d'abord présenter des caractéristiques mécaniques satisfaisantes pour réaliser par usinage des pièces présentant les dimensions et la rigidité souhaités de façon à pouvoir atteindre, sans déformation, un vide généralement du niveau au moins du vide moyen (10" - 10" Torr ). Ainsi la résistance à rupture (Rm) souhaitée est généralement d'au moins 260 MPa et même d'avantage si possible. De plus les contraintes résiduelles dans les blocs destinés à être usinés dans la masse doivent être faibles de façon à atteindre les dimensions souhaitées sans difficulté et sans déformation à l'usinage. Les dimensions des chambres à vide augmentant de façon continue, notamment pour la réalisation de panneaux à cristaux liquide ou de panneaux photovoltaïques de grande dimension, il est nécessaire de réaliser des blocs en alliage d'aluminium de plus en plus épais, notamment d'au moins 250 mm ou même 300 mm d'épaisseur. Plus les blocs sont épais, plus il est difficile d'obtenir des propriétés mécaniques suffisantes en maintenant une excellente stabilité à l'usinage. Indeed, the blocks must first have satisfactory mechanical characteristics to achieve by machining parts having the desired dimensions and rigidity so as to reach, without deformation, a vacuum generally at least the level of the average vacuum (10 " - 10 " Torr). Thus the desired breaking strength (R m ) is generally at least 260 MPa and even more preferably if possible. In addition, the residual stresses in the blocks intended to be machined in the mass must be low so as to reach the desired dimensions without difficulty and without deformation during machining. Since the dimensions of the vacuum chambers increase continuously, especially for the production of liquid crystal panels or large photovoltaic panels, it is necessary to produce increasingly thick aluminum alloy blocks, particularly from minus 250 mm or even 300 mm thick. The thicker the blocks, the more difficult it is to obtain sufficient mechanical properties while maintaining excellent machining stability.
Le niveau de porosité des blocs doit par ailleurs être suffisamment faible pour atteindre si nécessaire le haut-vide (10 6 - 10"8 Torr). De plus, les gaz utilisés dans les chambres à vide sont fréquemment très réactifs et de façon à éviter les risques de pollution des plaquettes de silicium ou des dispositifs à cristaux liquides par des particules ou des substances provenant des parois des chambres à vide et/ou un remplacement fréquent des pièces, il est important de protéger les surfaces des chambres. L'aluminium s'avère être un matériau avantageux à ce point de vue car il est en général possible de réaliser par anodisation une couche d'oxyde dure en surface des blocs, résistante aux gaz réactifs. Cependant, la résistance de la couche anodique est affectée par de nombreux facteurs liés notamment à la microstructure du produit (taille de grains, précipitation des phases, porosité) et il est toujours souhaitable d'améliorer ce paramètre. The level of porosity of the blocks must also be low enough to reach the high-vacuum (10 6 - 10 "8 Torr) if necessary, and the gases used in the vacuum chambers are frequently very reactive and so as to avoid the risks of pollution of silicon wafers or liquid crystal devices by particles or substances from the walls of vacuum chambers and / or frequent replacement of parts, it is important to protect the surfaces of the rooms. 'proves to be a material advantageous from this point of view because it is generally possible to perform anodizing a hard oxide layer on the surface of the blocks, resistant to reactive gases. However, the strength of the anodic layer is affected by many factors related in particular to the microstructure of the product (grain size, phase precipitation, porosity) and it is always desirable to improve this parameter.
Enfin, comme pour tout procédé industriel, il est souhaitable d'atteindre les propriétés visées par un procédé économique. Le développement à grande échelle des chambres à vide pour de nombreuses applications de grandes distribution (écrans plats, panneaux solaires) a récemment accru l'intérêt pour la simplification des procédés de fabrication.  Finally, as with any industrial process, it is desirable to achieve the properties targeted by an economic process. The large-scale development of vacuum chambers for many large distribution applications (flat screens, solar panels) has recently increased interest in simplifying manufacturing processes.
Le brevet US 6,565,984 (Applied Materials Inc.) décrit un alliage adapté à la fabrication des chambres pour fabrication de semi-conducteur de composition (en % en poids) Si : 0,54 - 0,74; Cu : 0,15-0,30; Fe : 0;05 - 0;20 ; Mn < 0,14 ; Zn < 0,15 ; Cr : 0,16 - 0,28 ; Ti < 0,06 ; Mg : 0 ,9 - 1,1. Les pièces sont obtenues par extrusion ou, usinage jusqu'à la forme désirée. La composition permet un contrôle de la taille des particules d'impuretés ce qui améliore la performance de la couche anodique.  U.S. Patent No. 6,565,984 (Applied Materials Inc.) discloses an alloy suitable for the manufacture of semiconductor manufacturing chambers of composition (in% by weight) Si: 0.54 - 0.74; Cu: 0.15-0.30; Fe: 0; 05 - 0; 20; Mn <0.14; Zn <0.15; Cr: 0.16 - 0.28; Ti <0.06; Mg: 0.9-1.1. The pieces are obtained by extrusion or machining to the desired shape. The composition makes it possible to control the size of the impurity particles, which improves the performance of the anodic layer.
Le brevet US 6,982,121 (Kyushyu Mitsui Aluminum) décrit un alliage adapté à anodisation et adapté aux chambres pour traitement plasma contenant (en % en poids) Mg : 2,0 à 3,5 ; Ti : 0,004 à 0,01 % et le reste aluminium de pureté 99,9%. L'alliage ne nécessite pas de traitement thermique contrairement aux alliages nécessitant la précipitation de Mg2Si. De plus, l'alliage ne nécessite pas la présence de Cr et de Mn qui doivent être ajoutés aux alliages 5052 et 6061 pour contrôler la taille de grain, mais qui risquent de provoquer des pollutions en métaux lourds des semi-conducteurs traités. Les caractéristiques mécaniques de l'alliage ne sont cependant pas indiquées. Par ailleurs le coût de l'aluminium de pureté 99,9 % est élevé. No. 6,982,121 (Kyushyu Mitsui Aluminum) discloses an alloy suitable for anodizing and adapted to plasma treatment chambers containing (in% by weight) Mg: 2.0 to 3.5; Ti: 0.004 to 0.01% and the remaining aluminum of purity 99.9%. The alloy does not require heat treatment, unlike alloys requiring the precipitation of Mg 2 Si. In addition, the alloy does not require the presence of Cr and Mn which must be added to alloys 5052 and 6061 to control the size of the alloy. grain, but which may cause pollution of heavy metals treated semiconductors. The mechanical characteristics of the alloy are however not indicated. Moreover, the cost of 99.9% pure aluminum is high.
La demande de brevet US 2009/0050485 (Kobe Steel, Ltd.) décrit un alliage de composition (en % en poids) Mg : 0, 1 - 2,0 ; Si : 0,1 - 2,0 ; Mn : 0,1 - 2,0 ; Fe, Cr, and Cu < 0,03, anodisé de façon à ce que la dureté de la couche d'oxyde anodique varie dans l'épaisseur. La très faible teneur en fer, chrome et cuivre entraine un surcoût important pour le métal utilisé.  US Patent Application 2009/0050485 (Kobe Steel, Ltd.) discloses a composition alloy (in% by weight) Mg: 0.1 - 2.0; If: 0.1 - 2.0; Mn: 0.1 - 2.0; Fe, Cr, and Cu <0.03, anodized so that the hardness of the anodic oxide layer varies in thickness. The very low content of iron, chromium and copper leads to a significant additional cost for the metal used.
Les demandes de brevet US 2001/019777 et JP2001 220637 (Kobe Steel) décrivent un alliage pour chambres comprenant (en % en poids) Si : 0,1 - 2,0, Mg : 0,1 - 3,5, Cu : 0,02-4,0 et des impuretés, la teneur en Cr étant inférieure à 0,04 %. Ces documents divulguent en particulier des produits obtenus en réalisant avant mise en solution une étape de laminage à chaud. La demande de brevet EP 2 003 219 A2 (Kobe Steel) décrit un alliage de forgeage comprenant ( en % en poids) Mg 0,5 - 1,25%, Si : 0,4 - 1,4% , Cu : 0,01 - 0,7%, Fe : 0,05 - 0,4%, Mn : 0,001 - 1,0%, Cr 0,01 - 0,35%, Ti et Zr 0,005 - 0,1% . Ce document divulgue en particulier des produits obtenus en réalisant avant mise en solution une étape de forgeage à chaud. The patent applications US 2001/019777 and JP2001 220637 (Kobe Steel) disclose an alloy for chambers comprising (in% by weight) Si: 0.1 - 2.0, Mg: 0.1 - 3.5, Cu: 0 , 02-4.0 and impurities, the Cr content being less than 0.04%. In particular, these documents disclose products obtained by performing a hot rolling step prior to dissolving. The patent application EP 2 003 219 A2 (Kobe Steel) describes a forging alloy comprising (in% by weight) Mg 0.5 - 1.25%, Si: 0.4 - 1.4%, Cu: 0, 01 - 0.7%, Fe: 0.05 - 0.4%, Mn: 0.001 - 1.0%, Cr 0.01 - 0.35%, Ti and Zr 0.005 - 0.1%. In particular, this document discloses products obtained by performing a hot forging step prior to dissolution.
Le document " The effect of processing and Mn content on the T5 and T6 properties of AA6082 profiles ", Journal of Materials Processing Technology, 173 (2006) 84-91 décrit des profilés en alliage AA6082. Ce document divulgue en particulier des produits obtenus en réalisant avant mise en solution une étape de filage à chaud.  The document "The effect of processing and Mn content on the T5 and T6 properties of AA6082 profiles", Journal of Materials Processing Technology, 173 (2006) 84-91 discloses AA6082 alloy profiles. In particular, this document discloses products obtained by performing a hot-spinning step before putting into solution.
Les procédés utilisés dans ces documents conduisent à un coût élevé (pureté de l'aluminium utilisé, nombre d'étapes du procédé). Il existe un besoin pour un procédé amélioré et peu coûteux de fabrication de blocs en alliage d'aluminium destinées à être utilisés dans la réalisation des chambres à vide, présentant des caractéristiques mécaniques élevées, de faibles contraintes résiduelles et permettant après usinage la formation de couches anodiques résistantes aux gaz réactifs. The processes used in these documents lead to a high cost (purity of the aluminum used, number of process steps). There is a need for an improved and inexpensive method of manufacturing aluminum alloy blocks for use in making vacuum chambers, having high mechanical characteristics, low residual stresses and allowing after machining the formation of layers anodic resistant to reactive gases.
Objet de l'invention Object of the invention
Un premier objet de l'invention est un procédé de fabrication d'un bloc d'aluminium d'épaisseur au moins égale à 250 mm destiné à la fabrication d'éléments pour chambres à vide dans lequel, successivement,  A first object of the invention is a method of manufacturing an aluminum block with a thickness of at least 250 mm intended for the production of elements for vacuum chambers in which, successively,
(a) on coule par coulée semi-continue un bloc en alliage de composition, en % en poids, Si : 0,5 - 1,5 ; Mg : 0,5-1,5 ; Fe < 0,3 ; Cu < 0,2 ; Mn < 0,8 ; Cr < 0, 10 ; Ti < 0,15; autres éléments < 0,05 chacun et < 0,15 au total, reste aluminium ;  (a) casting a composition alloy block, in% by weight, Si: 0.5 - 1.5; Mg: 0.5-1.5; Fe <0.3; Cu <0.2; Mn <0.8; Cr <0.10; Ti <0.15; other elements <0.05 each and <0.15 in total, remaining aluminum;
(b) optionnellement, on réalise une homogénéisation du bloc coulé à une température comprise entre 500 °C et 590 °C ;  (b) optionally, the cast block is homogenized at a temperature between 500 ° C and 590 ° C;
(c) on réalise un traitement thermique de mise en solution à une température comprise entre 450 °C et 560 °C directement sur le bloc coulé et optionnellement homogénéisé, sans réaliser avant mise en solution d'étape de déformation à chaud ou à froid ;  (c) a solution heat treatment is carried out at a temperature of between 450 ° C. and 560 ° C. directly on the cast block and optionally homogenized, without producing a hot or cold deformation step solution beforehand;
(d) on trempe le bloc ainsi mis en solution avec une vitesse de refroidissement entre la température de mise en solution et 200 °C au moins égale à 200 °C/h ;  (d) the block thus dissolved is quenched with a cooling rate between the solution temperature and 200 ° C at least equal to 200 ° C / h;
(e) optionnellement on détensionne le bloc ainsi trempé ; (f) on réalise le revenu du bloc ainsi trempé et optionnellement détensionné. (e) optionally, the block thus quenched is stripped; (f) the income of the block thus hardened and optionally relieved is realized.
Un autre objet de l'invention est une bloc de composition, en % en poids, Si : 0,5 - 1,5 ; Mg : 0,5-1,5 ; Fe < 0,3 ; Cu < 0,2 ; Mn < 0,8 ; Cr < 0,10 ; Ti < 0,15 autres éléments < 0,05 chacun et < 0,15 au total, reste aluminium, d'épaisseur au moins égale à 250 mm, et présentant à l'état T6 ou T652 une résistance à rupture Rm à ¼ épaisseur au moins égale à 280 MPa et une limite d'élasticité Rpo,2 à ¼ épaisseur au moins égale à 240 MPa, obtenu par coulée semi- continue, optionnellement homogénéisation du bloc coulé à une température comprise entre 500 °C et 590 °C , mise en solution à une température comprise entre 450 °C et 560 °C directement sur le bloc coulé et optionnellement homogénéisé, sans réaliser avant mise en solution d'étape de déformation à chaud ou à froid, trempe avec une vitesse de refroidissement entre la température de mise en solution et 200 °C au moins égale à 200 °C/h, optionnellement détensionnement et revenu. Encore un autre objet de l'invention est l'utilisation d'une bloc selon l'invention dans la réalisation de chambres à vide pour la fabrication de circuits électroniques intégrés à base de semi-conducteurs, d'écrans d'affichage plats et/ou que de panneaux photo voltaïques. Another subject of the invention is a block of composition, in% by weight, Si: 0.5 - 1.5; Mg: 0.5-1.5; Fe <0.3; Cu <0.2; Mn <0.8; Cr <0.10; Ti <0.15 other elements <0.05 each and <0.15 in total, remains aluminum, with a thickness of at least 250 mm, and having, in the T6 or T652 state, a breaking strength R m at ¼ thickness at least equal to 280 MPa and an elastic limit R p o, 2 to ¼ thickness at least equal to 240 MPa, obtained by semi-continuous casting, optionally homogenization of the cast block at a temperature between 500 ° C and 590 ° C., dissolved at a temperature of between 450 ° C. and 560 ° C. directly on the cast block and optionally homogenized, without producing a hot or cold deformation step solution, quenching with a cooling rate between the dissolution temperature and 200 ° C at least equal to 200 ° C / h, optionally stress relief and income. Yet another object of the invention is the use of a block according to the invention in the production of vacuum chambers for the manufacture of integrated electronic circuits based on semiconductors, flat display screens and / or or that of photovoltaic panels.
Description des figures Description of figures
Figure 1 : Structure granulaire des blocs obtenus par le procédé selon l'invention 11 (FIGla) et 21 (FIGlb). Figure 1: Granular structure of the blocks obtained by the process according to the invention 11 (FIGla) and 21 (FIGlb).
Figure 2 : Structure granulaire du bloc de référence 31 (FIG2a) et du bloc obtenu par un procédé selon l'art antérieur (déformation par fofgeage avant mise en solution) (FIG2b). Description détaillée de l'invention  FIG. 2: Granular structure of the reference block 31 (FIG. 2a) and of the block obtained by a method according to the prior art (deformation by fofage before dissolution) (FIG. 2b). Detailed description of the invention
La désignation des alliages se fait en conformité avec les règlements de The Aluminium Association (AA), connus de l'homme du métier. Les définitions des états métallurgiques sont indiquées dans la norme européenne EN 515. The designation of the alloys is in accordance with the regulations of The Aluminum Association (AA), known to those skilled in the art. The definitions of the metallurgical states are given in the European standard EN 515.
Sauf mention contraire, les caractéristiques mécaniques statiques, en d'autres termes la résistance à la rupture Rm, la limite d'élasticité conventionnelle à 0,2% d'allongement Rp0,2 et l'allongement à la rupture A%, sont déterminées par un essai de traction selon la norme EN 10002-1, le prélèvement et le sens de l'essai étant définis par la norme EN 485-1. La dureté est mesurée selon la norme EN ISO 6506. Les éléments pour chambre à vide sont notamment des corps de chambres à vide, des corps de vanne, des brides, des éléments de connexion, des éléments d'étanchéité, des passages, des tuyaux flexibles. Unless otherwise stated, the static mechanical characteristics, in other words the ultimate tensile strength Rm, the conventional yield stress at 0.2% elongation Rp0.2 and the elongation at break A%, are determined by a tensile test according to EN 10002-1, the sampling and the direction of the test being defined by EN 485-1. Hardness is measured according to EN ISO 6506. The elements for vacuum chamber include vacuum chamber bodies, valve bodies, flanges, connecting elements, sealing elements, passages, flexible pipes.
Dans le procédé selon l'invention, un alliage de la famille 6xxx est transformé en bloc utilisable pour la réalisation d'éléments pour chambres à vide sans réaliser avant mise en solution d'étape de déformation à chaud ou à froid. Ainsi, selon l'invention, un bloc d'épaisseur au moins égale à 250 mm en alliage de composition (en % en poids) Si : 0,5 - 1,5 ; Mg : 0,5-1,5 ; Fe < 0,3 ; Cu < 0,2 ; Mn < 0,8 ; Cr < 0,10 ; Ti < 0,15 ; autres éléments < 0,05 chacun et < 0,15 au total, reste aluminium est obtenu par coulée semi-continue, optionnellement homogénéisation du bloc coulé à une température comprise entre 500 °C et 590 °C ; mise en solution à une température comprise entre 450 et 560 °C directement sur le bloc coulé et optionnellement homogénéisé, sans réaliser avant mise en solution d'étape de déformation à chaud ou à froid; trempe avec une vitesse de refroidissement entre la température de mise en solution et 200 °C au moins égale à 200 °C/h ; optionnellement détensionnement et revenu. Par mise en solution directement sur le bloc coulé, sans réaliser avant mise en solution d'étape de déformation à chaud ou à froid, on entend dans le cadre de la présente invention qu'il n'est pas réalisé d'étape de déformation à chaud ou à froid avant la mise en solution, cependant des étapes classiques telles que l'usinage de surface ou le sciage d'extrémité peuvent être réalisées, notamment avant ou après l'homogénéisation.  In the process according to the invention, an alloy of the 6xxx family is converted into a block that can be used for the production of elements for vacuum chambers without producing a hot or cold deformation step solution before being put into solution. Thus, according to the invention, a block of thickness at least equal to 250 mm of alloy composition (in% by weight) Si: 0.5 - 1.5; Mg: 0.5-1.5; Fe <0.3; Cu <0.2; Mn <0.8; Cr <0.10; Ti <0.15; other elements <0.05 each and <0.15 in total, aluminum remains is obtained by semi-continuous casting, optionally homogenization of the cast block at a temperature between 500 ° C and 590 ° C; dissolving at a temperature of between 450 and 560 ° C. directly on the cast block and optionally homogenized, without producing before putting into solution the deformation step under hot or cold conditions; quenching with a cooling rate between the solution temperature and 200 ° C at least 200 ° C / h; optionally stress relief and income. By putting into solution directly on the cast block, without realizing before putting into solution of hot or cold deformation step, it is meant in the context of the present invention that no deformation step is carried out at hot or cold before the dissolution, however, conventional steps such as surface machining or end sawing can be performed, especially before or after homogenization.
La teneur en fer doit être inférieure à 0,3 % en poids car au-delà de cette valeur la couche anodique obtenue pour protéger le métal des gaz réactifs n'atteint pas la résistance souhaitée. Les présents inventeurs ont constaté cependant qu'il n'est pas nécessaire d'atteindre un niveau de pureté très élevé pour obtenir des couches anodiques présentant les caractéristiques souhaitées avec le procédé selon l'invention. Ainsi, la teneur en fer est de manière avantageuse d'au moins 0,1 % en poids, ce qui rend le procédé selon l'invention particulièrement économique. The iron content must be less than 0.3% by weight because beyond this value, the anodic layer obtained to protect the metal from the reactive gases does not reach the desired resistance. The present inventors have found, however, that it is not necessary to achieve a very high level of purity to obtain anodic layers having the desired characteristics with the process according to the invention. Thus, the iron content is advantageously at least 0.1% by weight, which makes the process according to the invention particularly economical.
La teneur en cuivre doit être inférieure à 0,2 % en poids car une teneur en cuivre trop élevée augmente la sensibilité à la trempe. Il est cependant avantageux dans certains cas d'ajouter une quantité limitée de cuivre pour améliorer les caractéristiques mécaniques, notamment lorsque la vitesse de refroidissement après mise en solution est supérieure à 800 °C/h. Une teneur en cuivre comprise entre 0,03 et 0,15 % en poids est préférée dans un mode de réalisation de l'invention. Les présents inventeurs ont constaté que si la teneur en chrome n'est pas inférieure à 0,10 % en poids, les propriétés mécaniques souhaitées, notamment la résistance mécanique minimale, ne sont pas atteintes. Il est communément admis que pour la réalisation d'un produit corroyé pour chambre à vide en alliage de la famille 6xxx la présence de chrome et/ou de manganèse est nécessaire de façon à contrôler la taille de grain. Les présents inventeurs ont constaté que dans le cadre de la présente invention, l'absence de chrome est au contraire favorable car sans dégrader la structure granulaire elle permet de limiter la sensibilité à la trempe et d'améliorer les caractéristiques mécaniques des produits épais. Dans un mode de réalisation avantageux de l'invention, la teneur en chrome est inférieure à 0,05 % en poids et de préférence inférieure à 0,03% en poids. La teneur en manganèse doit quant à elle être inférieure à 0,8 % en poids, une teneur supérieure à 0,8 % en poids étant néfaste notamment en ce qui concerne les propriétés de la couche anodique et la contamination de la chambre à vide. Avantageusement la teneur en manganèse est inférieure à 0,6 % en poids pour éviter la formation de phases grossières pouvant être nocives pour les propriétés de la couche anodique. Dans une réalisation avantageuse de l'invention, la teneur en manganèse est même inférieure à 0,05 % en poids. Les présents inventeurs ont constaté que de manière surprenante, même en l'absence de Cr, Mn et Zr, la structure granulaire obtenue par le procédé selon l'invention est contrôlée et permet d'obtenir des caractéristiques satisfaisantes en termes de propriétés mécaniques et de résistance aux gaz réactifs. L'absence simultanée de Cr, Mn et Zr permet ainsi de diminuer très significativement la sensibilité à la trempe de l'alliage et donc d'améliorer les propriétés mécaniques des produits épais, sans pour autant dégrader les caractéristiques granulaires et les propriétés des couches anodiques. Dans un mode de réalisation avantageux de l'invention, les teneurs en Cr, Mn et Zr sont simultanément inférieures à 0,05 % en poids et de manière préférée inférieures à 0,03 % en poids. The copper content must be less than 0.2% by weight because a too high copper content increases the quenching sensitivity. It is however advantageous in some cases to add a limited amount of copper to improve the mechanical characteristics, especially when the cooling rate after dissolution is greater than 800 ° C / h. A copper content of between 0.03 and 0.15% by weight is preferred in one embodiment of the invention. The present inventors have found that if the chromium content is not less than 0.10% by weight, the desired mechanical properties, in particular the minimum mechanical strength, are not achieved. It is commonly accepted that for the realization of a wrought product for the 6xxx family vacuum chamber the presence of chromium and / or manganese is necessary in order to control the grain size. The present inventors have found that in the context of the present invention, the absence of chromium is on the contrary favorable because without degrading the granular structure it makes it possible to limit the sensitivity to quenching and to improve the mechanical characteristics of the thick products. In an advantageous embodiment of the invention, the chromium content is less than 0.05% by weight and preferably less than 0.03% by weight. The manganese content must in turn be less than 0.8% by weight, a content greater than 0.8% by weight being detrimental especially with regard to the properties of the anodic layer and the contamination of the vacuum chamber. Advantageously, the manganese content is less than 0.6% by weight to prevent the formation of coarse phases which may be harmful for the properties of the anodic layer. In an advantageous embodiment of the invention, the manganese content is even less than 0.05% by weight. The present inventors have found that, surprisingly, even in the absence of Cr, Mn and Zr, the granular structure obtained by the process according to the invention is controlled and makes it possible to obtain satisfactory characteristics in terms of mechanical properties and resistance to reactive gases. The simultaneous absence of Cr, Mn and Zr thus makes it possible to very significantly reduce the sensitivity to quenching of the alloy and thus to improve the mechanical properties of the thick products, without degrading the granular characteristics and the properties of the anodic layers. . In an advantageous embodiment of the invention, the contents of Cr, Mn and Zr are simultaneously less than 0.05% by weight and preferably less than 0.03% by weight.
Les teneurs en silicium et en magnésium sont comprises entre 0,5 et 1,5 % en poids. D'une manière avantageuse, on réalise soit la combinaison de 0,5 à 0,8 % en poids de silicium avec 0,8 à 1 ,2 % en poids de magnésium, soit la combinaison de 0,8 à 1,2 % en poids de silicium avec 0,6 à 1,0 % en poids de magnésium. Dans une réalisation préférée de l'invention permettant d'atteindre des caractéristiques mécaniques particulièrement élevées, la teneur en silicium est comprise entre 0,8 et 1 % en poids et de préférence entre 0,85 et 0,95 % en poids et la teneur en magnésium est comprise entre 0,6 et 0,8 % en poids et de préférence entre 0,65 et 0,75 % en poids. La coulée de l'alliage est réalisée par coulée semi-continue avec refroidissement direct sous forme de bloc. Typiquement, on utilise un format de bloc ayant une épaisseur comprise entre 300 et 450 mm. The silicon and magnesium contents are between 0.5 and 1.5% by weight. Advantageously, the combination of 0.5 to 0.8% by weight of silicon with 0.8 to 1.2% by weight of magnesium or the combination of 0.8 to 1.2% is produced. by weight of silicon with 0.6 to 1.0% by weight of magnesium. In a preferred embodiment of the invention for achieving particularly high mechanical characteristics, the silicon content is between 0.8 and 1% by weight and preferably between 0.85 and 0.95% by weight and the content magnesium is between 0.6 and 0.8% by weight and preferably between 0.65 and 0.75% by weight. The casting of the alloy is carried out by semi-continuous casting with direct cooling in block form. Typically, a block format having a thickness between 300 and 450 mm is used.
Le bloc coulé peut optionnellement être homogénéisé à une température comprise entre 500 °C et 590 °C pendant au moins une heure. La réalisation d'une homogénéisation est avantageuse car elle permet généralement d'atteindre des propriétés mécaniques plus avantageuses et de meilleures propriétés de la couche anodique et par ailleurs de réduire la durée de mise en solution. L'homogénéisation peut être réalisée au cours d'un traitement thermique séparé ou alternativement au cours du traitement thermique de mise en solution.  The cast block may optionally be homogenized at a temperature between 500 ° C and 590 ° C for at least one hour. Achieving homogenization is advantageous because it generally makes it possible to achieve more advantageous mechanical properties and better properties of the anodic layer and also to reduce the dissolution time. The homogenization can be carried out during a separate heat treatment or alternatively during the solution heat treatment.
Entre la coulée et le traitement thermique de mise en solution, avant ou après l'homogénéisation quand celle -ci est pratiquée, on réalise en général un usinage de la surface (aussi appelé « scalpage ») de l'ordre d'au moins 5 mm par face, de façon à éliminer la couche ségrégée en surface et éviter la présence de fissures.  Between the casting and the solution heat treatment, before or after the homogenization when it is practiced, it is generally carried out a surface machining (also called "scalping") of the order of at least 5 mm per face, so as to eliminate the segregated layer on the surface and avoid the presence of cracks.
On réalise ensuite un traitement thermique de mise en solution directement sur le bloc coulé et optionnellement homogénéisé à une température comprise entre 450 et 560 °C, et de préférence entre 520 et 550 °C directement sans étape de déformation à chaud ou à froid préalable. Les déformations à chaud classiquement des procédés de l'art antérieur sont en général réalisées par laminage et/ou forgeage et/ou filage. Ainsi le bloc ne subit pas entre la coulée et la mise en solution d'étape de déformation significative par corroyage. Par corroyage on entend typiquement des opérations de laminage et/ou forgeage et/ou filage. Ainsi, selon l'invention, aucune des dimensions du bloc coulé (longueur, largeur, épaisseur) ne subit de modification significative, c'est-à-dire typiquement d'au moins environ 10% par corroyage entre la coulée et la mise en solution. La durée de mise en solution est de préférence supérieure à une heure. Le procédé selon l'invention, qui permet d'éviter la déformation à chaud ou à froid avant mise en solution est particulièrement avantageux d'un point de vue économique car cette étape est coûteuse. Selon l'art antérieur, ce type de procédé n'avait pas été envisagé notamment pour des blocs destinés à la réalisation d'éléments pour chambres à vide en alliage 6xxx, probablement car on craignait que, sans déformation à chaud, les caractéristiques mécaniques, la résistance des couches anodiques et le niveau de porosité, nécessaires pour fabriquer des éléments pour chambre à vide, ne soient pas atteintes. De plus, certains produits particulièrement épais n'étaient pas accessibles par les procédés selon l'art antérieur. De manière surprenante, les présents inventeurs ont constaté que le procédé ainsi simplifié permet non seulement d'atteindre des propriétés équivalentes à celles obtenues par le procédé selon l'art antérieur, mais dans certains cas de les dépasser. Après mise en solution, l'étape de trempe est critique, et doit être réalisée avec une vitesse de refroidissement entre la température de mise en solution et 200 °C au moins égale à 200 °C/h. La vitesse de refroidissement est calculée à mi-épaisseur des blocs. Si la vitesse de refroidissement est trop faible, les présents inventeurs ont constaté que les propriétés mécaniques recherchées ne sont pas atteintes. A solution heat treatment is then carried out directly on the cast block and optionally homogenized at a temperature of between 450 and 560 ° C., and preferably between 520 and 550 ° C. directly without a prior hot or cold deformation step. Hot deformations conventionally of the processes of the prior art are generally carried out by rolling and / or forging and / or spinning. Thus the block does not undergo between the casting and the setting solution of significant deformation step by wrought. Spinning is typically understood to mean rolling and / or forging and / or spinning operations. Thus, according to the invention, none of the dimensions of the cast block (length, width, thickness) undergo significant modification, that is to say typically at least about 10% by wrought between the casting and the implementation. solution. The dissolution time is preferably greater than one hour. The method according to the invention, which avoids hot or cold deformation before dissolution is particularly advantageous from an economic point of view because this step is expensive. According to the prior art, this type of process was not envisaged especially for blocks intended for the realization of elements for 6xxx alloy vacuum chambers, probably because it was feared that, without heat deformation, the mechanical characteristics, the resistance of the anode layers and the level of porosity necessary to make elements for vacuum chamber are not achieved. In addition, some particularly thick products were not accessible by the methods according to the prior art. Surprisingly, the present inventors have found that the method thus simplified not only makes it possible to achieve properties equivalent to those obtained by the method according to the prior art, but in certain cases to exceed them. After dissolution, the quenching step is critical, and must be performed with a cooling rate between the solution temperature and 200 ° C at least equal to 200 ° C / h. The cooling rate is calculated at the mid-thickness of the blocks. If the cooling rate is too low, the present inventors have found that the desired mechanical properties are not achieved.
Dans un premier mode de réalisation avantageux de l'invention, la vitesse de refroidissement est comprise entre 200 °C/h et 400 °C/h. En effet, de manière surprenante, lorsque la vitesse de refroidissement est comprise entre 200 °C/h et 400 °C/h, on obtient simultanément des caractéristiques mécaniques satisfaisantes et une faible énergie résiduelle permettant d'éviter l'étape de détensionnement par compression. Une telle vitesse de refroidissement peut être obtenue à l'aide d'une aspersion par un brouillard.  In a first advantageous embodiment of the invention, the cooling rate is between 200 ° C / h and 400 ° C / h. In fact, surprisingly, when the cooling rate is between 200 ° C./h and 400 ° C./h, satisfactory mechanical characteristics and a low residual energy are obtained at the same time, making it possible to avoid the compression stressing step. . Such a cooling rate can be obtained by means of mist spray.
Dans un second mode de réalisation avantageux de l'invention, la vitesse de refroidissement est au moins égale à 800 °C/h. Une telle vitesse de refroidissement peut être obtenue par aspersion ou immersion à l'eau. Une vitesse de refroidissement trop élevée pouvant générer des contraintes internes trop importantes dans les blocs, on utilise de préférence de l'eau à une température d'au moins 50 °C pour le refroidissement.  In a second advantageous embodiment of the invention, the cooling rate is at least 800 ° C./h. Such a cooling rate can be obtained by spraying or immersion in water. Since a cooling rate that is too high can generate excessive internal stresses in the blocks, it is preferable to use water at a temperature of at least 50 ° C. for cooling.
Optionnellement on détensionne le bloc ainsi trempé, de préférence par compression à froid avec un taux de déformation permanente compris entre 1 % et 5 %.. Dans le second mode de réalisation pour lequel la vitesse de refroidissement est supérieure à 800 °C/h, le détensionnement s'avère particulièrement avantageux. Le détensionnement permet de diminuer les contraintes résiduelles dans le métal et d'éviter les déformations lors de l'usinage.  Optionally the block thus hardened is stripped, preferably by cold compression with a permanent deformation rate of between 1% and 5%. In the second embodiment, for which the cooling rate is greater than 800 ° C./h, stress relief is particularly advantageous. The stress relieving allows to reduce the residual stresses in the metal and to avoid the deformations during the machining.
Enfin, on réalise le revenu du bloc ainsi trempé et optionnellement détensionné. La température de revenu est de préférence comprise entre 150 et 190 °C et de manière préférée entre 165 et 185°C, la durée de revenu étant comprise entre 5 et 40 heures et de manière préférée entre 8 et 20 heures. Avantageusement, on réalise un revenu pour atteindre l'état T6 ou T652, correspondant au pic des propriétés mécaniques statiques (Rm et Rpo,2). Finally, we realize the income of the block soaked and optionally relieved. The tempering temperature is preferably between 150 and 190 ° C and preferably between 165 and 185 ° C, the duration of income being between 5 and 40 hours and preferably between 8 and 20 hours. Advantageously, an income is obtained to reach the T6 or T652 state, corresponding to the peak of the static mechanical properties (R m and R p o, 2 ).
Les blocs obtenus par le procédé selon l'invention se caractérisent par des propriétés mécaniques élevées. Ainsi la résistance à rupture Rm à ¼ épaisseur des produits obtenus par le procédé selon l'invention est au moins égale à 280 MPa et la limite d'élasticité Rpo,2 à ¼ épaisseur est au moins égale à 240 MPa à l'état T6 ou T652. Dans un mode de réalisation avantageux, on utilise un alliage de composition Si : 0,5 - 1,2 ; Mg : 0,6-1,0 ; Fe 0, 1 - 0,3 ; Cu < 0,2 ; Mn < 0,05 ; Cr < 0,05 ; Ti < 0,15 ; autres éléments < 0,05 chacun et < 0, 15 au total, et on atteint à l'état T6 ou T652 une résistance à rupture Rm à ¼ épaisseur au moins égale à 300 MPa et une limite d'élasticité Rpo,2 à ¼ épaisseur est au moins égale à 270 MPa, et de plus si , la teneur en silicium est comprise entre 0,8 et 1 % en poids et de préférence entre 0,85 et 0,95 % en poids et la teneur en magnésium est comprise entre 0,6 et 0,8 % en poids et de préférence entre 0,65 et 0,75 % en poids, une résistance à rupture Rm à ¼ épaisseur au moins égale à 320 MPa et une limite d'élasticité Rp0,2 à ¼ épaisseur est au moins égale à 300 MPa, à l'état T6 ou T652. The blocks obtained by the process according to the invention are characterized by high mechanical properties. Thus the tensile strength R m at ¼ thickness of the products obtained by the process according to the invention is at least equal to 280 MPa and the yield strength R p o, 2 at ¼ thickness is at least equal to 240 MPa at 1 T6 or T652 state. In an advantageous embodiment, an alloy of composition Si: 0.5 - 1.2; Mg 0.6-1.0; Fe 0, 1 - 0.3; Cu <0.2; Mn <0.05; Cr <0.05; Ti <0.15; other elements <0.05 each and <0.15 in total, and in the T6 or T652 state a breaking strength R m is obtained at ¼ thickness of at least 300 MPa and an elastic limit R p o, 2 to ¼ thickness is at least equal to 270 MPa, and more if the silicon content is between 0.8 and 1% by weight and preferably between 0.85 and 0.95% by weight and the magnesium content is between 0.6 and 0.8% by weight and preferably between 0.65 and 0.75% by weight, a rupture strength R m at ¼ thickness at less than 320 MPa and a yield strength R p0.2 at ¼ thickness is at least equal to 300 MPa in the T6 or T652 state.
Une valeur minimale d'allongement, d'au moins 0,5 % est atteinte par les produits selon l'invention à l'état T6 ou T652. Dans certains cas une valeur minimale d'allongement d'au moins 4% est atteinte par les produits selon l'invention.  A minimum value of elongation of at least 0.5% is reached by the products according to the invention in the T6 or T652 state. In some cases a minimum elongation value of at least 4% is reached by the products according to the invention.
La structure granulaire des produits selon l'invention est caractéristique de l'absence de corroyage avant mise en solution. Ainsi il est possible de distinguer les produits selon l'invention des produits selon l'art antérieur pour lesquels une déformation à chaud ou à froid est réalisée avant la mise en solution par un simple examen métallographique. Typiquement, la structure granulaire des produits selon l'invention est isotrope, avec une taille de grain moyenne au moins égale à 200 μπι.  The granular structure of the products according to the invention is characteristic of the absence of wrought before dissolution. Thus it is possible to distinguish the products according to the invention of the products according to the prior art for which hot or cold deformation is performed before the dissolution in solution by a simple metallographic examination. Typically, the granular structure of the products according to the invention is isotropic, with an average grain size of at least 200 μπι.
Les blocs obtenus par le procédé selon l'invention sont aptes à être utilisés dans la réalisation de chambres à vide pour la fabrication de circuits électroniques intégrés à base de semiconducteurs, d'écrans d'affichage plats et/ou de panneaux photovoltaïques. Ainsi, le comportement à l'usinage des blocs est favorable, grâce notamment aux caractéristiques mécaniques élevées et au faible niveau de contraintes résiduelles. De plus les couches anodiques obtenues sur les blocs usinés par les procédés usuels d'anodisation sont résistantes aux gaz réactifs utilisés dans les chambres à vide. Les blocs obtenus par le procédé selon l'invention peuvent également être avantageusement utilisés pour tout autre application dans laquelle les propriétés obtenues sont favorables. The blocks obtained by the process according to the invention are suitable for use in the production of vacuum chambers for the manufacture of integrated electronic circuits based on semiconductors, flat display screens and / or photovoltaic panels. Thus, the machining behavior of the blocks is favorable, thanks in particular to the high mechanical characteristics and the low level of residual stresses. In addition, the anode layers obtained on the blocks machined by the usual anodizing processes are resistant to the reactive gases used in the vacuum chambers. The blocks obtained by the process according to the invention can also be advantageously used for any other application in which the properties obtained are favorable.
Exemple Dans cet exemple on a comparé le procédé selon l'invention avec un procédé selon des exemples de référence. Le procédé selon l'invention a été appliqué à deux alliages différents. On a coulé, par coulée semi-continue à refroidissement direct, quatre blocs en alliage dont la composition est donnée dans le tableau 1. Les blocs ont été scalpés jusqu'à l'épaisseur 410 mm. Tableau 1. Composition des alliages testés (% en poids) Example In this example the process according to the invention was compared with a method according to reference examples. The process according to the invention has been applied to two different alloys. Four alloy blocks, the composition of which is given in Table 1, were cast by direct-cooling semi-continuous casting. The blocks were scalped to a thickness of 410 mm. Table 1. Composition of the alloys tested (% by weight)
Les blocs ont été homogénéisés à une température comprise entre 540 et 590 °C pendant une durée d'au moins 4 heures. The blocks were homogenized at a temperature between 540 and 590 ° C for a period of at least 4 hours.
Les blocs ont ensuite été mis en solution à 540 °C. Après mise en solution, les blocs 11, 21 et 31 ont été trempés avec de l'eau à 60 °C (la vitesse de refroidissement moyenne calculée entre The blocks were then dissolved at 540 ° C. After dissolution, the blocks 11, 21 and 31 were quenched with water at 60 ° C. (the average cooling rate calculated between
540 °C et 200 °C était de environ 1500 °C/h), tandis que le bloc 12 a été trempé avec de l'air la vitesse de refroidissement moyenne entre 540 °C et 200 °C était d'environ 90 °C/h. 540 ° C and 200 ° C was about 1500 ° C / h), while the block 12 was quenched with air the average cooling rate between 540 ° C and 200 ° C was about 90 ° C / h.
Les différents blocs ont ensuite subi une compression à froid de 1,5 à 2,5% puis ont subi un revenu à 165 °C de façon à obtenir un état T652.  The different blocks then underwent a cold compression of 1.5 to 2.5% and then experienced an income at 165 ° C so as to obtain a T652 state.
La structure granulaire des produits obtenus est présentée sur les Figure la (bloc 11), lb (bloc The granular structure of the products obtained is shown in Figure la (block 11), lb (block
21) et 2a (bloc 31). Pour comparaison, la structure granulaire d'un produit par un procédé selon l'art antérieur (forgeage avant mise en solution) est présentée sur la figure 2b. 21) and 2a (block 31). For comparison, the granular structure of a product by a method according to the prior art (forging before dissolution) is presented in FIG. 2b.
Les caractéristiques mécaniques obtenues sont fournies dans le tableau 2  The mechanical characteristics obtained are given in Table 2
Tableau 2 : caractéristiques mécaniques obtenues (état T652) après prélèvement à ¼ épaisseur dans la direction TL. Table 2: Mechanical characteristics obtained (T652 state) after sampling at ¼ thickness in the TL direction.
31 (Ref) 276 229 6,2 87 31 (Ref) 276 229 6.2 87
12 (Ref) 159 92 16,2  12 (Ref) 159 92 16.2
Les blocs obtenus par le procédé selon l'invention (11 et 21), présentent un résistance mécanique (Rm, Rp0,2) plus élevée que celle obtenue avec les lingots de référence, la résistance mécanique obtenue avec le lingot 11 étant particulièrement avantageuse. The blocks obtained by the process according to the invention (11 and 21), have a higher mechanical strength (Rm, Rp0,2) than that obtained with the reference ingots, the mechanical strength obtained with the ingot 11 being particularly advantageous.
Les blocs obtenus selon l'invention présentaient de faibles contraintes résiduelles ce qui permet d'éviter la déformation des blocs lors de l'usinage. Le niveau de porosité observé dans les blocs selon l'invention était très faible, suffisamment faible pour atteindre le haut-vide. The blocks obtained according to the invention had low residual stresses which avoids the deformation of the blocks during machining. The level of porosity observed in the blocks according to the invention was very low, sufficiently low to reach high-vacuum.

Claims

Revendications claims
1. Procédé de fabrication d'un bloc d'aluminium d'épaisseur au moins égale à 250 mm destiné à la fabrication d'éléments pour chambres à vide dans lequel, successivement,  1. A method of manufacturing an aluminum block with a thickness of at least 250 mm intended for the production of elements for vacuum chambers in which, successively,
(a) on coule par coulée semi-continue un bloc en alliage de composition, en % en poids, Si : 0,5 - 1 ,5 ; Mg : 0,5-1,5 ; Fe < 0,3 ; Cu < 0,2 ; Mn < 0,8 ; Cr < 0,10 ; Ti < 0,15; autres éléments < 0,05 chacun et < 0,15 au total, reste aluminium ;  (a) casting a composition alloy block, in% by weight, Si: 0.5 - 1, 5; Mg: 0.5-1.5; Fe <0.3; Cu <0.2; Mn <0.8; Cr <0.10; Ti <0.15; other elements <0.05 each and <0.15 in total, remaining aluminum;
(b) optionnellement, on réalise une homogénéisation du bloc coulé à une température comprise entre 500 °C et 590 °C ;  (b) optionally, the cast block is homogenized at a temperature between 500 ° C and 590 ° C;
(c) on réalise un traitement thermique de mise en solution à une température comprise entre 450 et 560 °C directement sur le bloc coulé et optionnellement homogénéisé, sans réaliser avant mise en solution d'étape de déformation à chaud ou à froid;  (C) a solution heat treatment is carried out at a temperature of between 450 and 560 ° C. directly on the cast block and optionally homogenized, without carrying out a hot or cold deformation step before solution;
(d) on trempe le bloc ainsi mis en solution avec une vitesse de refroidissement entre la température de mise en solution et 200 °C au moins égale à 200 °C/h ;  (d) the block thus dissolved is quenched with a cooling rate between the solution temperature and 200 ° C at least equal to 200 ° C / h;
(e) optionnellement on détensionne le bloc ainsi trempé ;  (e) optionally, the block thus quenched is stripped;
(f) on réalise le revenu du bloc ainsi trempé et optionnellement détensionné. (f) the income of the block thus hardened and optionally relieved is realized.
2. Procédé selon la revendication 1 dans lequel la teneur en manganèse est inférieure à 0,6 % en poids et de préférence inférieure à 0,05 % en poids2. Method according to claim 1 wherein the manganese content is less than 0.6% by weight and preferably less than 0.05% by weight
3. Procédé selon la revendication 1 ou la revendication 2 dans lequel la teneur en chrome est inférieure à 0,05 % en poids et de préférence inférieure à 0,03% en poids. 3. A process according to claim 1 or claim 2 wherein the chromium content is less than 0.05% by weight and preferably less than 0.03% by weight.
4. Procédé selon une quelconque des revendications 1 à 3 dans lequel les teneurs en Cr, Mn et Zr sont simultanément inférieures à 0,05 % en poids et de manière préférée inférieures à 0,03 % en poids. 4. Method according to any one of claims 1 to 3 wherein the contents of Cr, Mn and Zr are simultaneously less than 0.05% by weight and preferably less than 0.03% by weight.
5. Procédé selon une quelconque des revendications 1 à 4 dans lequel la teneur en fer est d'au moins 0,1 % en poids. The process of any one of claims 1 to 4 wherein the iron content is at least 0.1% by weight.
6. Procédé selon une quelconque des revendications 1 à 5 dans lequel la teneur en silicium est de 0,5 à 0,8 % en poids et la teneur en magnésium est de 0,8 à 1,2 % en poids. 6. A process according to any one of claims 1 to 5 wherein the silicon content is 0.5 to 0.8% by weight and the magnesium content is 0.8 to 1.2% by weight.
7. Procédé selon une quelconque des revendications 1 à 5 dans lequel la teneur en silicium est de 0,8 à 1 ,2 % en poids et la teneur en magnésium est de 0,6 à 1,0 % en poids. The method of any of claims 1 to 5 wherein the silicon content is 0.8 to 1.2 wt.% And the magnesium content is 0.6 to 1.0 wt.%.
8. Procédé selon la revendication 7 dans lequel la teneur en silicium est comprise entre 0,8 et 1 % en poids et de préférence entre 0,85 et 0,95 % en poids et la teneur en magnésium est comprise entre 0,6 et 0,8 % en poids et de préférence entre 0,65 et 0,75 % en poids. 8. The method of claim 7 wherein the silicon content is between 0.8 and 1% by weight and preferably between 0.85 and 0.95% by weight and the magnesium content is between 0.6 and 0.8% by weight and preferably between 0.65 and 0.75% by weight.
9. Procédé selon une quelconque des revendications 1 à 8 dans lequel ladite vitesse de refroidissement entre la température de mise en solution et 200 °C est comprise entre 200 °C/h et 400 °C/h. 9. A process according to any one of claims 1 to 8 wherein said cooling rate between the solution temperature and 200 ° C is between 200 ° C / h and 400 ° C / h.
10. Procédé selon une quelconque des revendications 1 à 8 dans lequel ladite vitesse de refroidissement entre la température de mise en solution et 200 °C est au moins égale à 800 °C/h. 10. Process according to any one of claims 1 to 8 wherein said cooling rate between the solution temperature and 200 ° C is at least equal to 800 ° C / h.
11. Procédé selon une quelconque des revendications 1 à 10 dans lequel le détensionnement est effectué par compression à froid avec un taux de déformation permanente compris entre 1 % et 5 %. 11. Method according to any one of claims 1 to 10 wherein the stress relieving is performed by cold compression with a permanent deformation rate of between 1% and 5%.
12. Bloc de composition, en % en poids, Si : 0,5 - 1,5 ; Mg : 0,5-1,5 ; Fe < 0,3 ; Cu < 0,2 ; Mn < 0,8 ; Cr < 0,10 ; Ti < 0, 15 autres éléments < 0,05 chacun et < 0,15 au total, reste aluminium, d'épaisseur au moins égale à 250 mm, et présentant à l'état T6 ou T652 une résistance à rupture Rm à ¼ épaisseur au moins égale à 280 MPa et une limite d'élasticité Rpo,2 à ¼ épaisseur est au moins égale à 240 MPa , obtenu par coulée semi-continue, optionnellement homogénéisation du bloc coulé à une température comprise entre 500 °C et 590 °C ; mise en solution à une température comprise entre 450 et 560 °C directement sur le bloc coulé et optionnellement homogénéisé sans réaliser avant mise en solution d'étape de déformation à chaud ou à froid; trempe avec une vitesse de refroidissement entre la température de mise en solution et 200 °C au moins égale à 200 °C/h ; optionnellement détensionnement et revenu. 12. Block of composition, in% by weight, Si: 0.5 - 1.5; Mg: 0.5-1.5; Fe <0.3; Cu <0.2; Mn <0.8; Cr <0.10; Ti <0, 15 other elements <0.05 each and <0.15 in total, remains aluminum, with a thickness of at least 250 mm, and having, in the T6 or T652 state, a breaking strength R m at ¼ thickness at least equal to 280 MPa and a yield strength R p o, 2 to ¼ thickness is at least equal to 240 MPa, obtained by semi-continuous casting, optionally homogenization of the cast block at a temperature of between 500 ° C. and 590 ° C; dissolving at a temperature between 450 and 560 ° C directly on the cast block and optionally homogenized without performing before putting into solution of deformation step hot or cold; quenching with a cooling rate between the solution temperature and 200 ° C at least 200 ° C / h; optionally stress relief and income.
13. Bloc selon la revendication 12 obtenu par le procédé selon une quelconque des revendications 1 à 1 1. 13. Block according to claim 12 obtained by the method according to any one of claims 1 to 1 1.
14. Bloc selon la revendication 12 ou la revendication 13 caractérisé en ce que la composition est, en % en poids, Si : 0,5 - 1,2 ; Mg : 0,6-1,0 ; Fe 0,1 - 0,3 ; Cu < 0,2 ; Mn < 0,05 ; Cr < 0,05 ; Ti < 0,15 ; autres éléments < 0,05 chacun et < 0,15 au total, et en ce que à l'état T6 ou T652 la résistance à rupture Rm à ¼ épaisseur est au moins égale à 300 MPa et la limite d'élasticité Rp0,2 à ¼ épaisseur est au moins égale à 270 MPa. 14. Block according to claim 12 or claim 13 characterized in that the composition is, in% by weight, Si: 0.5 - 1.2; Mg 0.6-1.0; Fe 0.1 - 0.3; Cu <0.2; Mn < 0.05; Cr <0.05; Ti <0.15; other elements <0.05 each and <0.15 in total, and in the state T6 or T652 the breaking strength R m at ¼ thickness is at least 300 MPa and the yield strength R p0 , 2 to ¼ thickness is at least equal to 270 MPa.
15. Utilisation d'un bloc selon une quelconque des revendications 12 à 14 dans la réalisation de chambres à vide pour la fabrication de circuits électroniques intégrés à base de semi-conducteurs, d'écrans d'affichage plats et/ou que de panneaux photo voltaïques. 15. Use of a block according to any one of claims 12 to 14 in the production of vacuum chambers for the manufacture of integrated electronic circuits based on semiconductors, flat display screens and / or photo panels. voltaic.
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