EP2526216A1 - Verfahren zur herstellung von 6xxx-legierungsmaterialien für vakuumkammern - Google Patents

Verfahren zur herstellung von 6xxx-legierungsmaterialien für vakuumkammern

Info

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
Authority
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
Other languages
English (en)
French (fr)
Other versions
EP2526216B1 (de
Inventor
Cédric GASQUERES
Joost Vankappel
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.)
Constellium Valais AG
Constellium Issoire SAS
Original Assignee
Constellium Valais AG
Constellium France SAS
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 Constellium Valais AG, Constellium France SAS filed Critical Constellium Valais AG
Publication of EP2526216A1 publication Critical patent/EP2526216A1/de
Application granted granted Critical
Publication of EP2526216B1 publication Critical patent/EP2526216B1/de
Active legal-status Critical Current
Anticipated expiration legal-status Critical

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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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Conductive Materials (AREA)
  • Continuous Casting (AREA)
  • Heat Treatment Of Articles (AREA)
EP11706295.0A 2010-01-20 2011-01-18 Verfahren zur herstellung von 6xxx-legierungsmaterialien für vakuumkammern Active EP2526216B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US29659310P 2010-01-20 2010-01-20
FR1000212A FR2955336B1 (fr) 2010-01-20 2010-01-20 Procede de fabrication de produits en alliage 6xxx pour chambre a vide
PCT/FR2011/000029 WO2011089337A1 (fr) 2010-01-20 2011-01-18 Procédé de fabrication de produits en alliage 6xxx pour chambres à vide

Publications (2)

Publication Number Publication Date
EP2526216A1 true EP2526216A1 (de) 2012-11-28
EP2526216B1 EP2526216B1 (de) 2016-10-19

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EP11706295.0A Active EP2526216B1 (de) 2010-01-20 2011-01-18 Verfahren zur herstellung von 6xxx-legierungsmaterialien für vakuumkammern

Country Status (5)

Country Link
US (1) US20120325381A1 (de)
EP (1) EP2526216B1 (de)
JP (1) JP2013517383A (de)
FR (1) FR2955336B1 (de)
WO (1) WO2011089337A1 (de)

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FR2955336B1 (fr) 2013-02-15
WO2011089337A1 (fr) 2011-07-28
JP2013517383A (ja) 2013-05-16
US20120325381A1 (en) 2012-12-27
FR2955336A1 (fr) 2011-07-22
EP2526216B1 (de) 2016-10-19

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