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    • 专利摘要:
    The invention relates to a vacuum chamber element obtained by machining and surface treatment of a sheet of thickness at least equal to 10 mm of aluminum alloy composition, in% by weight, Si: 0.4 - 0 , 7; Mg: 0.4 - 1.0; the ratio in% by weight Mg / Si being less than 1.8; Ti: 0.01-0.15, Fe 0.08-0.25; Cu <0.35; Mn <0.4; Cr: <0.25; Zn <0.04; other elements <0.05 each and <0.15 in total, remains aluminum, characterized in that the grain size of said sheet is such that the average linear intercept length l, measured in the L / TC plane according to the ASTM E112 standard, is at least equal to 350 μm between surface and ½ thickness. The invention also relates to the method of manufacturing such a vacuum chamber element. The products according to the invention are particularly advantageous especially in terms of resistance to deformation by creep at high temperature, all having high properties of corrosion resistance, homogeneity of the properties in the thickness and the ability to 'machining.
    公开号:FR3063740A1
    申请号:FR1751981
    申请日:2017-03-10
    公开日:2018-09-14
    发明作者:Guillaume DELGRANGE；Christophe CHABRIOL；Romain-Fabrice Bernes
    申请人:Constellium Issoire SAS；
    IPC主号:
    专利说明:

    Holder (s): CONSTELLIUM ISSOIRE Simplified joint-stock company.
    Extension request (s)
    Agent (s): C-TEC CONSTELLIUM TECHNOLOGY CENTER.
    (54 / ELEMENTS OF VACUUM CHAMBERS IN ALUMINUM ALLOY STABLE AT HIGH TEMPERATURE.
    FR 3 063 740 - A1
    The invention relates to a vacuum chamber element obtained by machining and surface treatment of a sheet of thickness at least equal to 10 mm in aluminum alloy of composition, in% by weight, Si: 0.4 - 0 , 7; Mg: 0.4 -1.0; the ratio in% by weight Mg / Si being less than 1.8; Ti: 0.01 - 0.15, Fe 0.08 - 0.25; Cu <0.35; Mn <0.4; Cr: <0.25; Zn <0.04; other elements <0.05 each and <0.15 in total, remains aluminum, characterized in that the grain size of said sheet is such that the average length of linear interception I, measured in the plane L / TC according to the standard ASTM E112, is at least equal to 350 μm between surface and 1/2 thickness. The invention also relates to the method of manufacturing such a vacuum chamber element. The products according to the invention are particularly advantageous in particular in terms of resistance to deformation by creep at high temperature, while having high properties of resistance to corrosion, homogeneity of properties in thickness and ability to l 'machining.
    HIGH TEMPERATURE STABLE ALUMINUM ALLOY VACUUM CHAMBER ELEMENTS
    Field of the invention
    The invention relates to aluminum alloy products intended to be used as elements of vacuum chambers in particular for the manufacture of integrated electronic circuits based on semiconductors, flat display screens as well as photovoltaic panels and their manufacturing process.
    State of the art
    The elements of vacuum chambers for the manufacture of integrated electronic circuits based on semiconductors, flat display screens and photovoltaic panels can typically be obtained from aluminum alloy sheets.
    The vacuum chamber elements are elements intended for the manufacture of vacuum chamber structures and internal vacuum chamber components, in particular vacuum chamber bodies, valve bodies, flanges, connection elements, elements sealing, passages, diffusers, electrodes. They are obtained in particular by machining and surface treatment of aluminum alloy sheets.
    To obtain satisfactory vacuum chamber elements, aluminum alloy sheets must have certain properties.
    In fact, the sheets must first of all have satisfactory mechanical characteristics in order to produce by machining parts having the desired dimensions and rigidity so as to be able to reach, without deformation, a vacuum generally of at least the level of the average vacuum (10 3 - 10 5 Torr). Thus the desired breaking strength (R m ) is generally at least 260 MPa and even more if possible. In addition, to be able to be machined, the sheets intended to be machined in the mass must have homogeneous properties in the thickness and have a low density of stored elastic energy coming from residual stresses. In addition, in certain applications the vacuum chamber elements are subjected to high temperatures and it is important that their resistance to deformation by creep at high temperature is high.
    The level of porosity of the sheets must also be low enough to reach high vacuum (10 6 - 10 8 Torr) if necessary. In addition, the gases used in vacuum chambers are frequently very corrosive and so as to avoid the risks of pollution of silicon wafers or liquid crystal devices by particles or substances originating from the elements of vacuum chambers and / or frequent replacement of these elements, it is important to protect the surfaces of the vacuum chamber elements. Aluminum proves to be an advantageous material from this point of view because it is possible to carry out a surface treatment generating an oxide layer resistant to reactive gases. This surface treatment includes an anodization step and the oxide layer obtained is generally called anodic layer. In the context of the invention, the term “corrosion resistance” is understood more particularly to mean the resistance of anodized aluminum to corrosive gases used in vacuum chambers and to the corresponding tests. However, the protection provided by the anode layer is affected by many factors linked in particular to the microstructure of the sheet (size and shape of grains, phase precipitation, porosity) and it is always desirable to improve this parameter. Corrosion resistance is notably evaluated by the so-called “bubble test” which consists in measuring the duration of appearance of hydrogen bubbles on the surface of the anodized product during contact with a dilute solution of hydrochloric acid. The durations known in the prior art are of the order of tens of minutes to a few hours.
    To improve the vacuum chamber elements, it is possible to improve the aluminum sheets and / or the surface treatment carried out.
    US Patent 6,713,188 (Applied Materials Inc.) describes an alloy suitable for the manufacture of chambers for manufacturing a semiconductor with a composition (in% by weight) Si: 0.4 - 0.8; Cu: 0.15-0.30; Fe: 0; 001 - 0; 20; Mn 0.001 - 0.14; Zn 0.001 - 0.15; Cr: 0.04-0.28; Ti 0.001 - 0.06; Mg: 0.8 - 1.2. The parts are obtained by extrusion or machining to the desired shape. The composition allows control of the size of the impurity particles which improves the performance of the anode layer.
    US Patent 7,033,447 (Applied Materials Inc.) claims an alloy suitable for the manufacture of chambers for manufacturing a semiconductor with a composition (in% by weight) Mg: 3.5 - 4.0; Cu: 0.02 - 0.07; Mn: 0; 005 - 0; 015; Zn 0.08 - 0.16; Cr 0.02 - 0.07; Ti: 0 - 0.02; If <0.03; Fe <0.03. The parts are anodized in a solution comprising 10% to 20% by weight of sulfuric acid, 0.5 to 3% by weight of oxalic acid at a temperature of 7 to 21 ° C. The best result obtained in the bubble test is 20 hours.
    US Patent 6,686,053 (Kobe) claims an alloy having improved corrosion resistance, in which the anodic oxide comprises a barrier layer and a porous layer and in which at least part of the layer is altered to boehmite and / or pseudo -boehmite. The best result obtained in the bubble test is around 10 hours.
    The patent application US 2009/0050485 (Kobe Steel, Ltd.) describes an alloy of composition (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 US 2010/0018617 (Kobe Steel, Ltd.) describes an alloy of composition (in% by weight) Mg: 0.1 - 2.0; If: 0.1 - 2.0; Mn: 0.1 - 2.0; Fe, Cr, and Cu <0.03, the alloy being homogenized at a temperature above 550 ° C up to 600 ° C or below.
    Patent applications US 2001/019777 and JP2001 220637 (Kobe Steel) describe 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%. These documents disclose in particular products obtained by carrying out a hot rolling step before dissolution.
    International application WO2011 / 89337 (Constellium) describes a process for the production of non-laminated cast products suitable for the manufacture of vacuum chamber elements 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.
    US Patent 6,066,392 (Kobe Steel) describes an aluminum material having an anodic oxidation film with improved corrosion resistance, in which cracks are not generated even in high temperature thermal cycles and in environments corrosive.
    US Patent 6,027,629 (Kobe Steel) describes an improved surface treatment method for vacuum chamber elements in which the pore diameter of the anode layer is variable in the thickness thereof.
    US Patent 7,005,194 (Kobe Steel) describes an improved surface treatment method for vacuum chamber elements in which the anodized film is composed of a porous layer and a non-porous layer whose structure is at least partly boehmite or pseudo-boehmite.
    Patent application WO2014 / 060660 (Constellium France) relates to a vacuum chamber element obtained by machining and surface treatment of a sheet of thickness at least equal to 10 mm in aluminum alloy of composition, in% by weight , Si: 0.4-0.7;
    Mg: 0.4-0.7; Ti 0.01 - <0.15, Fe <0.25; Cu <0.04; Mn <0.4; Cr 0.01 - <0.1; Zn <0.04; other elements <0.05 each and <0.15 in total, aluminum remains.
    These documents do not mention the problem of improving the resistance to deformation by creep at high temperature.
    There is a need for further improved vacuum chamber elements, in particular in terms of resistance to creep deformation at high temperature, while maintaining high corrosion resistance properties, homogeneity of properties in thickness and machinability.
    Object of the invention
    A first object of the invention is a vacuum chamber element obtained by machining and surface treatment of a sheet of thickness at least equal to 10 mm in aluminum alloy of composition, in% by weight, Si: 0 , 4 - 0.7; Mg: 0.4 - 1.0; the ratio in% by weight Mg / Si being less than 1.8; Ti: 0.01 - 0.15, Fe 0.08 - 0.25; Cu <0.35; Mn <0.4; Cr: <0.25; Zn <0.04; other elements <0.05 each and <0.15 in total, remains aluminum, characterized in that the grain size of said sheet is such that the average length of linear interception £, measured in the plane L / TC measured according to ASTM standard El 12 is at least equal to 350 μm between surface and thickness.
    A second object of the invention is a method of manufacturing a vacuum chamber element in which successively
    at. an aluminum alloy rolling plate with a composition in% by weight, Si: 0.4-0.7; Mg: 0.4 - 1.0; the ratio in% by weight Mg / Si being less than 1.8; Ti: 0.01 - 0.15, Fe 0.08 - 0.25; Cu <0.35; Mn <0.4; Cr: <0.25; Zn <0.04; other elements <0.05 each and <0.15 in total, aluminum remains,
    b. optionally, said rolling plate is homogenized,
    vs. laminating said rolling plate at a temperature above 400 ° C to obtain a sheet of thickness at least equal to 10 mm,
    d. we carry out a solution treatment of said sheet, optionally preceded by a cold work hardening operation, and we quench it,
    e. said sheet is thus relieved in solution and quenched by controlled traction with a permanent elongation of 1 to 5%,
    f. an income is produced from the sheet metal thus pulled,
    g. optionally, an additional cold deformation of at least 3% is carried out and an annealing treatment at a temperature of at least 500 ° C., the annealing treatment can be carried out before or after steps h or i of machining and surface treatment,
    h. the sheet metal thus returned is machined into a vacuum chamber element,
    i. a surface treatment of the vacuum chamber element thus obtained is preferably carried out comprising an anodization carried out at a temperature between 10 and 30 ° C with a solution comprising 100 to 300 g / l of sulfuric acid and 10 to 30 g / l of oxalic acid and 5 to 30 g / l of at least one polyol, said process comprising steps of rolling and / or dissolving and / or additional cold deformation and annealing adapted to obtain a size of grain such as average linear intercept length f, measured in the L / TC plane according to the standard
    ASTM El 12, ie at least equal to 350 μm between surface and Vi thickness.
    Description of the figures
    FIG. 1 shows the granular structure of product A obtained in example 1 on L / TC sections after Barker attack.
    Figure 2 shows the geometry of the test piece used for the creep hot deformation tests.
    FIG. 3 shows the granular structure of the product F-1 (Figure 3A) and F-2 (Figure 3B) obtained in Example 2 on L / TC sections after Barker attack.
    FIG. 4 shows the granular structure of the products G and H obtained in Example 3 on L / TC sections after Barker attack, at the surface at% thickness and at Vi thickness.
    FIG. 5 shows the stress profile in thickness for the direction L of the products obtained in example 3.
    Detailed description of the invention
    The designation of the alloys is done in accordance with the regulations of The Aluminum Association (AA), known to those skilled in the art. The definitions of metallurgical states are given in European standard EN 515. Unless otherwise stated, the definitions of standard EN 12258-1 apply.
    Unless otherwise stated, the static mechanical characteristics, in other words the tensile strength Rm, the conventional elastic limit at 0.2% elongation Rp0.2 and the elongation at break A%, are determined by a tensile test according to standard ISO 6892-1, the sampling and the direction of the test being defined by standard EN 4851. The hardness is measured according to standard EN ISO 6506.
    The grain sizes are measured according to the ASTM El 12 standard. The average grain sizes are measured in the L / TC plane according to the intercept method of the standard (ASTM El 12-96 §16.3). The average length of linear interception is measured in the longitudinal direction f z (0 °) and the transverse direction / z (90 °). An average value in the plan
    L / TC /, called average length of linear interception in the L / TC plane, is calculated according to / = (/ z (o °) A z (90 °)) 1/2 · The anisotropy index A / z is calculated according to AI / = / z (0 °) / / / (90 °) · We also calculate the variation in the thickness of / z (90 °), A / z (90 °) according to the formula:
    Δ / z (90 °) = (max (/ z (90 °) (s, 'ΛΕρ / ζ, Ερ)) - min (/ z (90 °) (s,' ΛΕρ, 'ΛΕρ))) / avg (/ z (90 °) (s, 'ΛΕρ / Λ e p)) in which S: means Surface, U Ep means mid-thickness and N Ep means quarter-thickness.
    By surface grain size is meant in the context of the present invention the grain size measured after machining to remove 2 mm in the thickness direction. The breakdown voltage is measured according to standard EN ISO 2376: 2010.
    The present inventors have found that vacuum chamber elements having very advantageous properties in terms of resistance to deformation by creep at high temperature, while also having advantageous properties in terms of corrosion resistance, uniformity of properties and of machinability, are obtained for an aluminum alloy of the specific 6xxx series whose grain size is high and homogeneous in thickness compared to the products known according to the state of the art. A method of manufacturing a vacuum chamber element comprising steps for obtaining the grain size according to the invention has also been invented.
    The composition of the aluminum alloy sheets making it possible to obtain the vacuum chamber elements according to the invention is in% by weight, Si: 0.4 - 0.7; Mg: 0.4 - 1.0; the ratio in% by weight Mg / Si being less than 1.8; Ti: 0.01 - 0.15, Fe 0.08 - 0.25; Cu <0.35; Mn <0.4; Cr: <0.25; Zn <0.04; other elements <0.05 each and <0.15 in total, aluminum remains.
    The contents of these elements make it possible in particular to obtain, in combination with the grain size according to the invention, a high resistance to deformation in creep at high temperature.
    Magnesium and silicon are the major addition elements in the alloy products according to the invention. Their content was chosen with precision so as to achieve sufficient mechanical properties, in particular a tensile strength in the TL direction of at least 260 MPa and / or a yield strength in the TL direction of at least 200 MPa and also a homogeneous granular structure in thickness. The silicon content is between 0.4 and 0.7% by weight and preferably between 0.5% and 0.6% by weight. The magnesium content is between 0.4 and 1.0% by weight. Preferably the minimum magnesium content is 0.5% by weight. Preferably, the maximum content of magnesium is 0.7% by weight and preferably 0.6% by weight. In an advantageous embodiment, the magnesium content is from 0.4 to 0.7% by weight and preferably from 0.5 to 0.6% by weight. The preferred silicon and / or magnesium contents make it possible in particular to achieve, both at the surface and at mid-thickness, durations of appearance of hydrogen bubbles in the bubble test which are particularly remarkable for the products according to the invention. In addition, the ratio in% by weight Mg / Si must remain less than 1.8 and preferably less than 1.5. The present inventors have in fact found that if this ratio is too high, the resistance to creep deformation at high temperature decreases. The present inventors believe that too high a Mg content in solid solution could affect the resistance to creep deformation at high temperature.
    The present inventors have found that, surprisingly, too small an amount of iron affects the resistance to creep deformation at high temperature. Thus the minimum iron content is 0.08% by weight and preferably 0.10% by weight. Too much iron can adversely affect the properties of the anodic oxide layer. Thus the iron content is at most 0.25% by weight and preferably at most 0.20% by weight. In an advantageous embodiment of the invention, the iron content is from 0.10 to 0.20% by weight.
    The addition of too high a copper content may have an unfavorable effect on the resistance to creep deformation at high temperature. The copper content is therefore less than 0.35% by weight. In addition, a high copper content can degrade the properties of the protective oxide layer and / or contaminate the products produced in the vacuum chambers. Preferably the copper content is less than 0.05% by weight, preferably less than 0.02% by weight and more preferably less than 0.01% by weight.
    Too much titanium can also have a detrimental effect on the properties of the anodic oxide layer. Thus the titanium content is less than 0.15% by weight. However, the addition of a small amount of titanium has a favorable effect on the granular structure and its homogeneity, thus the titanium content is at least 0.01% by weight. In an advantageous embodiment of the invention, the titanium content is from 0.01 to 0.1% by weight and preferably from 0.01 to 0.05% by weight. Advantageously, the titanium content is at least 0.02% by weight and preferably at least 0.03% by weight.
    Too much chromium can also have a detrimental effect on the resistance to creep deformation at high temperature. Thus the chromium content is less than 0.25% by weight. However, the addition of a small amount of chromium can have a favorable effect on the granular structure, so the chromium content is preferably at least 0.01% by weight. In an advantageous embodiment of the invention, the chromium content is from 0.01 to 0.04% by weight and preferably from 0.01 to 0.03% by weight. The simultaneous addition of chromium and titanium is advantageous because it makes it possible in particular to improve the granular structure and in particular to reduce the anisotropy index of the grains.
    The control of the maximum contents of certain other elements is important because these elements can, if they are present in contents higher than those recommended, degrade the properties of the anodic oxide layer and / or contaminate the products manufactured in the empty. Thus, the manganese content is less than 0.4% by weight, preferably less than 0.04% by weight and preferably less than 0.02% by weight. The zinc content is less than 0.04% by weight, preferably less than 0.02% by weight and preferably less than 0.001% by weight.
    The aluminum alloy sheets according to the invention have a thickness of at least 10 mm. Advantageously, the aluminum alloy sheets according to the invention have a thickness of between 20 and 110 mm and preferably between 30 and 90 mm. In one embodiment of the invention, the aluminum alloy sheets according to the invention have a thickness of at least 50 mm and preferably at least 60 mm.
    The sheets according to the invention have a grain size such that the average length of linear interception measured in the plane L / TC according to standard ASTM El 12, is at least equal to 350 μm between surface and Vi thickness, and preferably at least equal to 400 μm between surface and Vi thickness, which contributes to obtaining a resistance to deformation in creep at high high temperature. Advantageously, the grain size is particularly homogeneous in thickness, and the sheet is such that the variation in thickness of the average length of linear interception in the L / TC plane in the transverse direction, called fz (90 °) according to standard ASTM El 12, is less than 30% and preferably less than 20%. The variation in grain size is calculated by taking the difference between the maximum and minimum value at Vi thickness,% thickness and area and dividing by the average of the values at Vi thickness,% thickness and area. Preferably, the average length of linear interception measured in the L / TC plane according to standard ASTM El 12 in the transverse direction fz (90 °) is at least equal to 200 μm and preferably at least equal to 230 μm between surface and Vi thickness.
    The sheets according to the invention have a resistance to deformation in creep at high temperature. Thus, advantageously, the creep deformation under a stress of 5 MPa at 420 ° C. is after 10 hours at most 0.40% and preferably at most 0.27%.
    The sheets according to the invention are suitable for machining. Thus the density of elastic energy stored
    Wtot, the measurement of which is described in Example 1, for the sheets according to the invention whose thickness is between 20 and 80 mm is advantageously less than 0.2 kJ / m 3 .
    The vacuum chamber elements according to the invention are obtained by a process in which
    at. an aluminum alloy rolling plate of composition according to the invention is poured,
    b. optionally, said rolling plate is homogenized,
    vs. laminating said rolling plate at a temperature above 400 ° C to obtain a sheet of thickness at least equal to 10 mm,
    d. we carry out a solution treatment of said sheet, optionally preceded by a cold work hardening operation, and we quench it,
    e. said sheet is thus relieved in solution and quenched by controlled traction with a permanent elongation of 1 to 5%,
    f. an income is produced from the sheet metal thus pulled,
    g. optionally, an additional cold deformation of at least 3% is carried out and an annealing treatment at a temperature of at least 500 ° C., the annealing treatment can be carried out before or after steps h or i of machining and surface treatment,
    h. the sheet metal thus returned is machined into a vacuum chamber element,
    i. a surface treatment of the vacuum chamber element thus obtained is carried out, preferably comprising an anodization carried out at a temperature between 10 and 30 ° C with a solution comprising 100 to 300 g / 1 of sulfuric acid and 10 to 30 g / 1 of oxalic acid and 5 to 30 g / 1 of at least one polyol, the process comprising steps of rolling and / or dissolving and / or additional cold deformation and annealing adapted to obtain a size of grain such as average length of linear interception f, measured in the plane L / TC according to standard ASTM El 12, that is to say at least equal to 350 μm between surface and Vi thickness.
    Homogenization is advantageous, it is preferably carried out at a temperature between 540 ° C and 600 ° C. Preferably, the homogenization time is at least 4 hours.
    When homogenization is carried out, the plate can be cooled after homogenization and then reheated before hot rolling or directly laminated after homogenization without intermediate cooling.
    Hot rolling conditions are important to obtain the desired microstructure, in particular to improve the corrosion resistance of the products. In particular, the rolling plate is maintained at a temperature above 400 ° C throughout the hot rolling. Preferably, the temperature of the metal is at least 450 ° C during hot rolling. The sheets according to the invention are laminated to a thickness of at least 10 mm.
    Then a solution dissolving treatment of the sheet optionally preceded by a cold work hardening operation, and it is quenched. The quenching can be carried out in particular by spraying or by immersion. The dissolution is preferably carried out at a temperature between 540 ° C and 600 ° C. Preferably, the duration of dissolution is at least 15 min, the duration being adapted as a function of the thickness of the products.
    The sheet thus dissolved is then tensioned by controlled traction with a permanent elongation of 1 to 5%.
    An income from the sheet thus pulled is then produced. The tempering temperature is advantageously between 150 ° C and 190 ° C. The duration of income is typically between 5h and 30h. Preferably, an income is achieved at the peak making it possible to reach a maximum elastic limit and / or a state T651.
    Optionally, an additional cold deformation of at least 3% is carried out and an annealing treatment at a temperature of at least 500 ° C., the annealing treatment can be carried out before or after the machining or surface treatment steps. .
    To obtain a grain size according to the invention, the steps of rolling and / or dissolving and / or additional cold deformation and annealing are adapted.
    In a first embodiment, the rolling temperature is maintained at a temperature above 500 ° C and preferably above 525 ° C during all the rolling steps. Advantageously in this first embodiment, the natural logarithm of the Zener-Hollomon parameter Z defined by equation (1), ln Z, is between 21 and 25 and preferably between 21.5 and 24.5 for the majority passes and preferably for all the passes carried out during hot rolling.
    Z = έ e Q / ( Rr > (1) where έ is the average strain rate in the thickness expressed in s 1 , Q is the activation energy of 156 kJ / mol, R is the constant of ideal gases 8.31 JK -1 mol -1 , T is the rolling temperature expressed in Kelvin.
    In this first embodiment, the last rolling pass is advantageously such that L / H is at least 0.6 where H is the thickness at the entrance to the rolling mill and L is the contact length in the rolling mill.
    In a second embodiment, the duration and / or the dissolution temperature are modified with respect to the duration and / or the dissolution temperature necessary to dissolve the alloying elements, so as to obtain a grain enlargement. Typically, the duration used is at least twice and / or the temperature is at least 10 ° C. higher than the duration and / or the dissolution temperature necessary for dissolving the alloying elements.
    In a third embodiment, the dissolution is preceded by a cold work hardening operation by rolling or traction with a deformation of at least 4% and preferably at least 7%.
    In a fourth embodiment, an additional cold deformation of at least 3% is carried out after the tempering step and an annealing treatment at a temperature of at least 500 ° C, and preferably at least 525 ° C, the annealing treatment can be carried out before or after the machining or surface treatment steps.
    The four embodiments can be combined to obtain the grain size according to the invention.
    A vacuum chamber element is obtained by machining and surface treatment of a sheet of thickness at least equal to 10 mm according to the invention.
    The surface treatment preferably comprises an anodization treatment to obtain an anodic layer whose thickness is typically between 20 and 80 μm.
    The surface treatment preferably comprises, before anodizing, degreasing and / or pickling with known products, typically alkaline products. Degreasing and / or pickling can include a neutralization operation, especially in the case of alkaline pickling, typically with an acidic product such as nitric acid, and / or at least one rinsing step.
    The anodization is carried out using an acid solution. It is advantageous for the surface treatment to include, after anodization, hydration (also called “clogging”) of the anodic layer thus obtained.
    In an advantageous embodiment, anodizing is carried out at a temperature between 10 and ° C with a solution comprising 100 to 300 g / 1 of sulfuric acid and 10 to 30 g / 1 of oxalic acid and 5 to 30 g / 1 at least one polyol and advantageously the product thus anodized is hydrated in deionized water at a temperature of at least 98 ° C, preferably for a period of at least about 1 hour. These advantageous anodization conditions make it possible to reach, both at the surface and at mid-thickness, durations of appearance of hydrogen bubbles in the test of particularly remarkable bubbles, in particular for the preferred products according to the invention, the content of which Mg is between 0.4 and 0.7% by weight, the Si content is between 0.4 and 0.7% by weight and the Cu content is less than 0.05% by weight for which the durations at the bubble test are preferably at least 750 min. Preferably, the aqueous solution used for the anodization of this advantageous surface treatment does not contain a titanium salt. The presence of at least one polyol in the anodizing solution also contributes to improving the corrosion resistance of the anodic layers. Ethylene glycol, propylene glycol or preferably glycerol are advantageous polyols. Anodizing is preferably carried out with a current density of between 1 and 5 A / dm 2 . The duration of anodization is determined so as to reach the desired anodic layer thickness.
    After anodization, it is advantageous to carry out a hydration step (also called clogging) of the anodic layer. Preferably the hydration is carried out in deionized water at a temperature of at least 98 ° C, preferably for a period of at least about 1 h. The present inventors have observed that it is particularly advantageous to carry out the hydration subsequent to the anodization in two stages in deionized water, a first stage lasting at least 10 min at a temperature of 20 to 70 ° C and a second step lasting at least about 1 hour at a temperature of at least 98 ° C. Advantageously, an anti-powder additive derived from triazine such as Anodal-SHl® is added to the deionized water used for the second stage of hydration.
    The vacuum chamber elements treated with the advantageous surface treatment process and obtained from sheets of which the thickness is between 20 and 80 mm easily reach at half-thickness a duration of appearance of hydrogen bubbles in a 5% hydrochloric acid solution ("bubble test") of at least about 400 min and preferably at least 750 min and even at least about 900 min, at least for the part corresponding to the surface of prison. The elements of vacuum chambers obtained from an alloy sheet according to the invention, the thickness of which is between 60 and 80 mm and with the advantageous surface treatment process can reach a duration on the surface of the sheet. appearance of hydrogen bubbles in a 5% hydrochloric acid solution at least 500 min and preferably at least 900 min at mid-thickness.
    The preferred products according to the invention whose Mg content is between 0.4 and 0.7% by weight, the Si content is between 0.4 and 0.7% by weight and the Cu content is lower at 0.05% by weight reach at mid-thickness a duration of appearance of hydrogen bubbles in a 5% hydrochloric acid solution (“bubble test”) of at least 750 min and a creep deformation under a stress of 5 MPa at 420 ° C is after 10 hours at most 0.27%.
    The use of vacuum chamber elements according to the invention in vacuum chambers is particularly advantageous because their properties are very homogeneous and, in particular for the anodized elements with the advantageous surface treatment process, the corrosion resistance is high which makes it possible to avoid pollution of the products manufactured in the rooms such as for example that the microprocessors or the slabs for flat screens.
    Examples
    Example 1
    In this example, 6xxx alloy sheets 16 mm thick have been prepared. Plates, the composition of which is given in Table 1, were cast.
    Table 1 - composition of alloys (% by weight)
    Alloy Yes Fe Cu Mn Mg Cr Ti Mg / Si A (Invention) 0.6 0.23 0.30 0.12 1.0 0.20 0.06 1.7 B (Reference) 0.6 0.23 0.29 0.12 1.2 0.20 0.07 2.0 C (Reference) 0.4 0.24 0.29 0.12 1.0 0.19 0.06 2.5 D (Reference) 0.6 0.07 0.29 0.12 1.0 0.20 0.06 1.7 E (Reference) 0.6 0.06 0.29 <0.01 1.0 0.30 0.06 1.7
    The plates were homogenized at a temperature of 560 ° C for 2 hours, hot-rolled to a thickness of 16 mm at a temperature of at least 400 ° C. The sheets thus obtained were dissolved for 2 hours at a temperature of 575 ° C (A,
    D, E), 545 ° C (C) or 570 ° C (B) adapted to their composition, hardened and pulled. The sheets obtained underwent a suitable income to reach a T651 state. The duration and the temperature of the dissolution were intended to obtain a grain size such as the average length of linear interception in the L / TC plane measured according to the ASTM standard.
    El 12, named f, ie at least equal to 350 μm between surface and Vi thickness. The micrograph obtained for sheet A, representative of all the sheets, is presented in Figure 1.
    The resistance to deformation by creep at high temperature was evaluated on test pieces as described in Figure 2, at a temperature of 420 ° C under a stress of 5 MPa. Deformation after 10 hours is provided in Table 2
    Table 2 - Deformation after 10 h of creep test at 420 ° C under a stress of 5 MPa.
    Alloy Deformation (%) A (Invention) 0.15 B (Reference) 0.29 C (Reference) 0.45 D (Reference) 0.46 E (Reference) 0.61
    Sheet A has undergone machining and surface treatment. In surface treatment, the product is degreased, pickled with an alkaline solution, then neutralized with a nitric acid solution before undergoing anodization at a temperature of around 20 ° C in a sulpho-oxalic bath. (sulfuric acid 160 g / 1 + oxalic acid 20g / l + 15 g / 1 glycerol). After anodization, a hydration treatment of the anodic layer is carried out in two stages: 20 min at 50 ° C in deionized water and then approximately 80 min in deionized water at boiling point in the presence of a derivative anti-powder additive. of triazine AnodalSH1®. The anode layer obtained was about 50 µm thick.
    The anode layer obtained was characterized by the following tests.
    The breakdown voltage characterizes the voltage at which a first electric current crosses the anode layer. The measurement method is described in standard EN ISO 2376: 2010. The value obtained was 2.6 kV.
    The "bubble test" is a corrosion test which characterizes the quality of the anode layer by measuring the duration of appearance of the first bubbles in a hydrochloric acid solution. A flat surface 20 mm in diameter of the sample is brought into contact at room temperature with a 5% by mass solution of HCl. The characteristic duration is the time from which a continuous flow of gas bubbles from at least one discrete point on the surface of the anodized aluminum is visible. The result was 450 minutes.
    Example 2
    In this example, alloy sheets of composition as indicated in Table 3 and with a thickness of 280 mm were prepared by homogenization and hot rolling at a temperature above 400 ° C.
    Table 3 - composition of the alloy (% by weight)
    Alloy Yes Fe Cu Mn Mg Cr Ti Mg / Si F 0.56 0.13 0.011 0.016 0.54 0.021 0.018 1
    One F-1 sheet was then pulled 8% while the other F-2 was not treated. The sheets thus obtained were dissolved for 6 hours at a temperature of 500 ° C. quenched and pulled. The sheets obtained underwent a suitable income to reach a T651 state.
    The granular structure of the various products obtained was observed at mid-thickness on L / TC sections by optical microscopy after Barker attack. The micrographs are presented in Figure 3A (sheet F1) and 3B (sheet F-2).
    The grain sizes measured in the L - TC plane are presented in table 4 table 4 - grain size in the L - TC plane (pm)
    Alloy Position f / (90 °)pm f / (0 °)pm i pm Ah(L / TC) Fl / 2 thickness 435 567 four hundred ninety seven 1.3 F2 / 2 thickness 223 359 283 1.6
    The resistance to deformation by creep at high temperature was evaluated on test pieces as described in Figure 2, at a temperature of 420 ° C under a stress of 5 MPa. Deformation after 10 hours is provided in Table 5.
    Table 5 - Deformation after 10 h of creep test at 420 ° C under a stress of 5 MPa.
    Alloy Deformation (%) F-l (Invention) 0.08% F-2 (Reference) 0.7%
    Example 3
    In this example, 6xxx alloy sheets with a thickness of 64 mm have been prepared. Plates, the composition of which is given in Table 6, were cast.
    Table 6 - composition of alloys (% by weight)
    Alloy Yes Fe Cu Mn Mg Cr Ti Mg / Si G 0.6 0.14 <0.01 <0.01 0.6 0.02 0.04 1.0 H 0.5 0.13 <0.01 <0.01 0.5 0.04 0.03 1.0
    The plates were homogenized at a temperature of 595 ° C for 12 hours.
    Plate G was hot rolled to a thickness of 64 mm at a temperature of at least 530 ° C and maintaining the Zener - Hollomon parameter for each rolling pass such that ln Z is between 22 and 24 , 5.
    Plate H was hot rolled to a thickness of 64 mm at a temperature of between 480 and 500 ° C., the Zener-Hollomon parameter being such that ln Z was greater than 26 for the majority of passes rolling.
    The sheets thus obtained were put in solution for 4 hours at a temperature of 535 ° C. and pulled by 3%. The sheets obtained underwent a suitable income to reach a T651 state.
    The mechanical properties in the TL direction were measured at quarter thickness and are reported in Table 7
    Table 7 - mechanical properties at quarter thickness in the TT direction
    Alloy Rp0.2(MPa) Rm(MPa) AT(%) G 268 289 7.2 H > 220 > 260 > 5
    Your resistance to deformation by creep at high temperature was evaluated on 5 test pieces as described in FIG. 2, at the temperature of 420 ° C. under a stress of 5 MPa. Deformation after 10 hours is provided in Table 8.
    Table 8 - Deformation after 10 h of creep test at 420 ° C under a stress of 5 MPa.
    Alloy Deformation (%) G 0.26% H 2.5%
    Your granular structure of the various products obtained was observed on T / TC sections by optical microscopy after Barker attack, on the surface at quarter and half thickness. Your micrographs are shown in Figure 4.
    The average grain sizes measured in the F / TC plan according to the intercept method of the standard (ASTM El 12-96 §16.3) are presented in Table 9.
    ableau 9 - grain size in the T - TC plane (pm)
    Alloy Position £ / (90 °)pm £ / (o °) ·pm £ pm Ah(L / TC) A £ / (90 °) G Area 246 770 435 3.1 14% % thickness 264 682 424 2.6 Z thickness 284 732 456 2.6 H Area 185 364 259 2.0 31% % thickness 226 688 394 3.0 / 2 thickness 254 738 433 2.9
    It is found that the product G according to the invention has a larger grain size than the product H and also more homogeneous in thickness.
    The residual stresses in the thickness were evaluated using the step-by-step method of machining rectangular bars taken in full thickness in the directions L and TL, described for example in the publication “Development of New Alloy for Distortion Free Machined Aluminum Aircraft Components ”, F. Heymes, B. Commet, B. Dubost, P. Fassince, P. Fequeu, GM. Raynaud, in l st International Non-Ferrous Processing & Technology Conference, 10-12 March 1997 - Adams's Mark Hotel, St Louis, Missouri. This method is mainly applied to plates whose length and width are significantly greater than the thickness and for which the residual stress state can be reasonably considered to be biaxial with its two main components in the directions L and T ( ie no residual stress in the direction S) and such that the level of residual stresses varies only in the direction S. This method is based on the measurement of the deformation of two rectangular bars of full thickness which are cut in the plate along L and TL directions. These bars are machined down in the direction S step by step, and at each step the deflection is measured, as well as the thickness of the machined bar.
    The width of the bar was 30 mm. The bar must be long enough to avoid any side effect on the measurements. A length of 400 mm was used.
    The measurements are made after each machining pass.
    After each machining pass, the bar is removed from the vice, and a stabilization time is observed before the deformation measurement is carried out, so as to obtain a uniform temperature in the bar after machining.
    At each step i, the thickness h (i) of each bar and the arrow f (i) of each bar are collected.
    These data make it possible to calculate the residual stress profile in the bar, corresponding to the stress c (î) l and to the stress c (î) lt as an average in the layer removed during the i step, given by the following formulas, in which E is the Young's modulus, If is the length between the supports used for the deflection measurement and vest the Poisson's ratio:
    from i = 1 to N-1 "or- / orl
    A 3 (z + 1)
    Zz (z) (Zz (z) - (Zz (z + 1))
    -S (i) L
    L * r
    V'T = ττΣ1 / <* +1 ) ι- / Wi yk = i
    - (/ z (z) + (/ z (z + l)) + h (k + ï) (3h (k) -h (k + ï)) 3h (k) u (i) L + vu (i ), T 1-v 2 ^ lt + vu (Ol
    1-v 2
    Finally, the elastic energy density stored in the Wtot bar can be calculated from the residual stress values using the following formulas:
    W tot = W L + W LT with
    500 v 1
    W L (kJ / m 3 ) = —- 2 σ Σ (ζ) [σ ζ (z) - νσ, -, (i) th (i)
    Ethfd
    500 v 1
    W LT (kJ / m 3 ) = —- 2 & LT (θ [σ ΖΓ (z) - νσ, (i)} th (i)
    Eth ~ 7
    The stress profile in the thickness for the direction L is given in figure 5. The total energy measured Wtot was 0.18 kJ / m 3 for sample G and 0.17 kJ / m 3 for l 'sample H.
    The products have undergone machining and surface treatment. In surface treatment, the product is degreased, pickled with an alkaline solution, then neutralized with a nitric acid solution before undergoing anodization at a temperature of around 20 ° C in a sulpho-oxalic bath. (sulfuric acid 160 g / 1 + oxalic acid 20g / l + 15 g / 1 glycerol). After anodization, a hydration treatment of the anodic layer is carried out in two stages: 20 min at 50 ° C in deionized water and then approximately 80 min in deionized water at boiling point in the presence of a derivative anti-powder additive. of triazine AnodalSH1®. The anode layer obtained was about 50 µm thick.
    The anode layers were characterized by the following tests.
    The breakdown voltage characterizes the voltage at which a first electric current crosses the anode layer. The measurement method is described in standard EN ISO 2376: 2010. The values are indicated in absolute value after measurement in direct current (DC).
    The "bubble test" is a corrosion test which characterizes the quality of the anode layer by measuring the duration of appearance of the first bubbles in a hydrochloric acid solution. A flat surface 20 mm in diameter of the sample is brought into contact at room temperature with a 5% by mass solution of HCl. The characteristic duration is the time from which a continuous flow of gas bubbles from at least one discrete point on the surface of the anodized aluminum is visible.
    The results measured at the surface and at mid-thickness are presented in Table 10.
    Table 10 - Characterization of the products after anodization
    Position Product Test ofbubbles(min) Breakdown voltage (KV) Area G 1020 2.0 H 1380 2.6 U thickness G > 1440 2.0 H > 1500 3.3 U thickness G 900 2.0 H 1320 2.8
    The product according to the invention has excellent properties after surface treatment.
    权利要求:
    Claims (13)
    [1" id="c-fr-0001]
    . Claims
    1. Vacuum chamber element obtained by machining and surface treatment of a sheet of thickness at least equal to 10 mm in aluminum alloy of composition, in% by weight,
    5 If: 0.4-0.7; Mg: 0.4 - 1.0; the ratio in% by weight Mg / Si being less than 1.8; Ti: 0.01 - 0.15, Fe 0.08 - 0.25; Cu <0.35; Mn <0.4; Cr: <0.25; Zn <0.04; other elements <0.05 each and <0.15 in total, remains aluminum, characterized in that the grain size of said sheet is such that the average length of linear interception €, measured in the plane
    L / TC according to standard ASTM El 12, is at least equal to 350 μm between surface and% thickness.
    [2" id="c-fr-0002]
    2. Element according to claim 1 characterized in that the grain size of said sheet is such that the variation in the thickness of the average length of linear interception in the plane L / TC in the transverse direction, called / (9o °) according to standard ASTM El 12, is less than 30% and preferably less than 20%.
    [3" id="c-fr-0003]
    3. Element according to claim 1 or claim 2 in which the creep deformation at the temperature of 420 ° C under a stress of 5 MPa is after 10 hours at most 0.40% and preferably at most 0.27 %.
    [4" id="c-fr-0004]
    4. Element according to any one of claims 1 to 3 wherein the magnesium content is from 0.4 to 0.7% by weight and preferably from 0.5 to 0.6% by weight.
    [5" id="c-fr-0005]
    5. Element according to any one of claims 1 to 4 wherein the copper content is less than 0.05% by weight, preferably less than 0.02% by weight and preferably less than 0.01% by weight.
    [6" id="c-fr-0006]
    6. Element according to any one of claims 1 to 5 wherein said sheet is such that its thickness is between 20 and 80 mm and its elastic energy density
    30 stored Wtot is less than 0.2 kJ / m 3 .
    [7" id="c-fr-0007]
    7. Element according to any one of claims 1 to 6 wherein said surface treatment comprises an anodization carried out at a temperature between 10 and 30 ° C with a solution comprising 100 to 300 g / 1 of sulfuric acid and 10 to 30 g / 1 of oxalic acid and 5 to 30 g / 1 of at least one polyol and in which said sheet is such that its thickness is between 20 and 80 mm that it has at mid-thickness a duration of appearance of hydrogen bubbles in a 5% hydrochloric acid solution greater than 400 min and preferably in which said sheet is such that its thickness is greater than 60 mm and has on the surface a duration of appearance of hydrogen bubbles in a 5% hydrochloric acid solution of at least 500 min.
    [8" id="c-fr-0008]
    8. Element according to claim 7, the Mg content of which is between 0.4 and 0.7% by weight, the Si content is between 0.4 and 0.7% by weight and the Cu content is lower. at 0.05% by weight of which at mid-thickness the duration of appearance of hydrogen bubbles in a 5% hydrochloric acid solution is at least at least 750 min and whose creep deformation under a stress of 5 MPa at 420 ° C is after 10 hours at most 0.27%.
    [9" id="c-fr-0009]
    9. Method of manufacturing a vacuum chamber element in which successively
    at. an aluminum alloy rolling plate with a composition in% by weight, Si: 0.4-0.7; Mg: 0.4 - 1.0; the ratio in% by weight Mg / Si being less than 1.8; Ti: 0.01 - 0.15, Fe 0.08 - 0.25; Cu <0.35; Mn <0.4; Cr: <0.25; Zn <0.04; other elements <0.05 each and <0.15 in total, aluminum remains,
    b. optionally, said rolling plate is homogenized,
    vs. laminating said rolling plate at a temperature above 400 ° C to obtain a sheet of thickness at least equal to 10 mm,
    d. we carry out a solution treatment of said sheet, optionally preceded by a cold work hardening operation, and we quench it,
    e. said sheet is thus relieved in solution and quenched by controlled traction with a permanent elongation of 1 to 5%,
    f. an income is produced from the sheet thus fractionated,
    g. optionally, an additional cold deformation of at least 3% is carried out and an annealing treatment at a temperature of at least 500 ° C., the annealing treatment can be carried out before or after steps h or i of machining and surface treatment,
    h. the sheet metal thus returned is machined into a vacuum chamber element,
    i. a surface treatment of the vacuum chamber element thus obtained is preferably carried out comprising an anodization carried out at a temperature between 10 and 30 ° C with a solution comprising 100 to 300 g / 1 of sulfuric acid and 10 to 30 g / 1 of oxalic acid and 5 to 30 g / 1 of at least one polyol, said process comprising steps of rolling and / or dissolving and / or additional cold deformation and annealing adapted to obtain a size of grain such as average linear intercept length f, measured in the L / TC plane according to the standard
    ASTM El 12, ie at least equal to 350 μm between surface and thickness.
    [10" id="c-fr-0010]
    10. The method of claim 9 wherein the rolling temperature is maintained at a temperature above 500 ° C and preferably at a temperature above 525 ° C.
    [11" id="c-fr-0011]
    11. The method of claim 10 wherein the natural logarithm of the Zener-Hollomon Z parameter defined by equation (1), ln Z, is between 21 and 25 and preferably between 21.5 and 24.5 for the majority of passes and preferably for all of the passes made during hot rolling.
    Z = è (1)
    [12" id="c-fr-0012]
    12. Method according to any one of claims 9 to 11 wherein the dissolution is preceded by a cold work hardening operation by rolling or traction with a deformation of at least 4% and preferably at least 7%.
    [13" id="c-fr-0013]
    13. Method according to any one of claims 9 to 12 in which an additional cold deformation of at least 3% is carried out after the tempering step and an annealing treatment at a temperature of at least 500 ° C, and preferably at least 525 ° C., the annealing treatment can be carried out before or after the machining and surface treatment steps.
    1/4
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    同族专利:
    公开号 | 公开日
    KR20190126851A|2019-11-12|
    SG11201907957YA|2019-11-28|
    US11248280B2|2022-02-15|
    CN110402296B|2021-04-20|
    FR3063740B1|2019-03-15|
    TW201840864A|2018-11-16|
    CN110402296A|2019-11-01|
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    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
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    FR2955336B1|2010-01-20|2013-02-15|Alcan Rhenalu|PROCESS FOR MANUFACTURING 6XXX ALLOY PRODUCTS FOR VACUUM CHAMBER|CN110129633B|2019-05-23|2020-06-05|江苏亨通电力特种导线有限公司|Aluminum alloy rivet line for furniture and preparation method thereof|
    FR3101641B1|2019-10-04|2022-01-21|Constellium Issoire|Aluminum alloy precision sheets|
    CN111041294B9|2019-12-31|2021-03-12|辽宁忠旺集团有限公司|6-series low alloy composition with high long-term thermal stability and preparation method thereof|
    CN113684400A|2021-08-22|2021-11-23|山东华建铝业科技有限公司|High-performance photovoltaic aluminum alloy frame and production process thereof|
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    优先权:
    申请号 | 申请日 | 专利标题
    FR1751981A|FR3063740B1|2017-03-10|2017-03-10|HIGH TEMPERATURE STABLE ALUMINUM ALLOY CHAMBER ELEMENTS|
    FR1751981|2017-03-10|FR1751981A| FR3063740B1|2017-03-10|2017-03-10|HIGH TEMPERATURE STABLE ALUMINUM ALLOY CHAMBER ELEMENTS|
    EP18714563.6A| EP3592875A1|2017-03-10|2018-03-01|Aluminium alloy vacuum chamber elements which are stable at high temperature|
    JP2019571109A| JP2020510761A|2017-03-10|2018-03-01|Aluminum alloy vacuum chamber element with high temperature stability|
    SG11201907957Y| SG11201907957YA|2017-03-10|2018-03-01|Aluminium alloy vacuum chamber elements stable at high temperature|
    PCT/FR2018/050481| WO2018162823A1|2017-03-10|2018-03-01|Aluminium alloy vacuum chamber elements which are stable at high temperature|
    US16/492,085| US11248280B2|2017-03-10|2018-03-01|Aluminium alloy vacuum chamber elements stable at high temperature|
    KR1020197029492A| KR20190126851A|2017-03-10|2018-03-01|High Temperature Stability Aluminum Alloy Vacuum Chamber Element|
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    TW107108171A| TW201840864A|2017-03-10|2018-03-09|Aluminium alloy vacuum chamber elements stable at high temperature|
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