CN114686787A - 6061 aluminum alloy containing granular iron-rich phase, preparation method thereof and gas distribution plate - Google Patents
6061 aluminum alloy containing granular iron-rich phase, preparation method thereof and gas distribution plate Download PDFInfo
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- CN114686787A CN114686787A CN202210322697.9A CN202210322697A CN114686787A CN 114686787 A CN114686787 A CN 114686787A CN 202210322697 A CN202210322697 A CN 202210322697A CN 114686787 A CN114686787 A CN 114686787A
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- 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
- C22F1/047—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 with magnesium as the next major constituent
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- 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
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- 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
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
Abstract
The invention provides a 6061 aluminum alloy containing a granular iron-rich phase, a preparation method thereof and a gas distribution plate, wherein the preparation method optimizes the preparation process flow by sequentially carrying out homogenization annealing, first preheating, forging, heat treatment annealing, second preheating, hot rolling, solution treatment, cold rolling and aging treatment on a 6061 aluminum alloy blank, can eliminate a lath-shaped iron-rich phase in the 6061 aluminum alloy, improves the corrosion resistance of the final 6061 aluminum alloy, can be used as the gas distribution plate, and has wide application prospect.
Description
Technical Field
The invention relates to the technical field of semiconductor part manufacturing, in particular to a 6061 aluminum alloy containing a granular iron-rich phase, a preparation method thereof and a gas distribution plate.
Background
The gas distribution plate is a common semiconductor component used in a reaction chamber of semiconductor equipment, and etching gas can uniformly reach the surface of a wafer after passing through the gas distribution plate, and reacts with the surface of the wafer to etch a required circuit pattern.
CN201066682Y discloses a gas distribution plate of semiconductor equipment, which comprises a plurality of gas injection pipes, each having a plurality of vent holes, wherein one of the gas injection pipes is installed at the center of the gas distribution plate. But does not address the issue of corrosion resistance of the gas distribution plate.
CN101898890A discloses an alumina ceramic for semiconductor equipment and a preparation process thereof, which adds a trace (300-3000ppm) of barium oxide without increasing the existing production cost, so that the sintered high-purity alumina ceramic is stable and uniform within the frequency range of 2MHz to 4.8GHz, does not change with the material batch and the position of the material blank after sintering, and is less than 3.0 x 10-4Dielectric loss coefficient of (2). The ceramic sintered body can be used for manufacturing various key parts of semiconductor vacuum manufacturing equipment, such as a gas nozzle, a gas distribution plate, a reaction chamber wall body, a fixing ring for fixing a wafer and the like of plasma equipment. But the ceramic material has high cost and is not suitable for large-scale popularization.
CN1489779A discloses a zirconia toughened ceramic component and coating in semiconductor processing equipment, which improves corrosion resistance by coating a layer of ceramic on the outer layer of a gas distribution plate, but the method is complicated to operate and has the problems of the bonding strength between the ceramic surface and the metal alloy, etc. which are difficult to popularize on a large scale.
At present, 6061 aluminum alloy is a commonly used material for a gas distribution plate, but at present, 6061 aluminum alloy is easy to cause chemical corrosion and influence the service performance of the material. Therefore, it is necessary to develop a new simple method for manufacturing the corrosion-resistant 6061 aluminum alloy.
Disclosure of Invention
In view of the problems in the prior art, the invention provides a 6061 aluminum alloy containing a granular iron-rich phase, a preparation method thereof and a gas distribution plate, wherein the preparation process flow is optimized, at least three forging processes are adopted after homogenization annealing, and hot rolling and cold rolling are sequentially carried out after heat treatment annealing, so that the problem of poor corrosion resistance of the 6061 aluminum alloy is solved, the electrochemical corrosion resistance of the gas distribution plate is improved, and the service life of the material is prolonged.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method of making a 6061 aluminum alloy containing a particulate iron-rich phase, the method comprising the steps of:
(1) carrying out homogenization annealing on the 6061 aluminum alloy blank to obtain a homogenized and annealed blank;
(2) forging the homogenized and annealed blank for at least three times after first preheating and first heat preservation to obtain a forged blank;
(3) carrying out heat treatment annealing on the forged blank to obtain a heat-treated and annealed blank;
(4) secondly preheating the blank subjected to the heat treatment annealing, carrying out second heat preservation, and then carrying out hot rolling to obtain a hot-rolled blank;
(5) the hot rolled blank is sequentially subjected to solution treatment and cooling, and then is subjected to cold rolling to obtain a cold rolled blank;
(6) and (3) sequentially carrying out aging treatment and leveling on the cold-rolled blank to obtain the 6061 aluminum alloy containing granular iron-rich phase.
The preparation method provided by the invention can obviously improve the corrosion performance of the 6061 aluminum alloy by carrying out homogenization annealing, first preheating, forging, heat treatment annealing, second preheating, hot rolling, solid solution treatment, cold rolling and aging treatment in sequence, wherein the sequence of the steps of homogenization treatment, forging, hot rolling and cold rolling is strictly controlled, and the technical principle is as follows: 6061 aluminum alloy contains iron impurities, and the original iron impurities can have the effect of refining grains, but in the casting process, aluminum, iron and silicon can generate a lath-shaped iron-rich phase, namely a lath-shaped AlFeSi phase, and the lath-shaped iron-rich phase can form a primary cell in aluminum, so that electrochemical corrosion is caused, and the service life and the use effect of the 6061 aluminum alloy are reduced; according to the invention, through the process flows which are sequentially carried out, the original lath-shaped iron-rich phase is converted into the granular iron-rich phase, so that the formation of a galvanic cell is avoided, and the effect of improving the corrosion resistance of the material is achieved.
Preferably, the temperature of the homogenizing annealing in the step (1) is 550 to 580 ℃, for example 550 ℃, 554 ℃, 557 ℃, 560 ℃, 564 ℃, 567 ℃, 570 ℃, 574 ℃, 577 ℃ or 580 ℃, etc., but not limited to the recited values, and other values not recited in the range are also applicable.
Preferably, the time for the homogenizing annealing in the step (1) is 12 to 24 hours, for example, 12 hours, 14 hours, 15 hours, 16 hours, 18 hours, 19 hours, 20 hours, 22 hours, 23 hours or 24 hours, etc., but not limited to the recited values, and other values not recited in the range are also applicable.
Preferably, the temperature of the first preheating in the step (2) is 400 to 500 ℃, for example, 400 ℃, 410 ℃, 420 ℃, 430 ℃, 440 ℃, 450 ℃, 460 ℃, 470 ℃, 480 ℃ or 500 ℃ and the like, but is not limited to the enumerated values, and other unrecited values in the range are also applicable.
Preferably, the first heat preservation time in step (2) is 5-30 min, such as 5min, 8min, 11min, 14min, 17min, 19min, 22min, 25min, 28min or 30min, but not limited to the values listed, and other values not listed in the range are also applicable.
Preferably, the first preheating in step (2) is performed in a heating furnace.
Preferably, the forging ratio in the single forging in the step (2) is 1.5 to 2.5, and may be, for example, 1.5, 1.7, 1.8, 1.9, 2, 2.1, 2.2, 2.3, 2.4 or 2.5, but not limited to the values listed, and other values not listed in this range are also applicable.
The forging ratio of the single forging is further preferably within the above range, and compared with other forging ratios, the forging ratio of the invention can not only ensure that the lath-shaped iron-rich phase does not appear, but also avoid the cracking and the like of the 6061 aluminum alloy.
Preferably, the temperature of the heat treatment annealing in the step (3) is 300 to 500 ℃, and for example, 300 ℃, 323 ℃, 345 ℃, 367 ℃, 389 ℃, 412 ℃, 434 ℃, 456 ℃, 478 ℃, or 500 ℃ may be used, but not limited to the recited values, and other values not recited in the range may be applied.
Preferably, the heat-treatment annealing in step (3) is performed for 60 to 180min, such as 60min, 70min, 80min, 100min, 110min, 120min, 140min, 150min, 160min or 180min, but not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
Preferably, the cooling manner after heat preservation in the heat treatment annealing in the step (3) includes water cooling.
Preferably, the temperature of the second preheating in the step (4) is 350 to 450 ℃, for example, 350 ℃, 360 ℃, 370 ℃, 380 ℃, 390 ℃, 400 ℃, 410 ℃, 420 ℃, 430 ℃ or 450 ℃, etc., but not limited to the recited values, and other values not recited in the range are also applicable.
Preferably, the time of the second heat preservation in the step (4) is 5-30 min, such as 5min, 8min, 11min, 10min, 15min, 19min, 20min, 25min, 28min or 30min, but not limited to the enumerated values, and other unrecited values in the range are also applicable.
Preferably, the second preheating in step (4) is performed in a heating furnace.
The hot rolling in step (4) preferably has a rolling deformation of 30 to 80%, and may be, for example, 30%, 36%, 42%, 47%, 53%, 58%, 64%, 69%, 75%, or 80%, but is not limited to the values listed above, and other values not listed above are also applicable.
Preferably, the rolling reduction per pass of the hot rolling in the step (4) is 19 to 21mm, for example, 19mm, 19.3mm, 19.5mm, 19.7mm, 19.9mm, 20.2mm, 20.4mm, 20.6mm, 20.8mm or 21mm, but not limited to the values listed, and other values not listed in the range are also applicable.
In the invention, the temperature, the reduction amount per pass and the rolling deformation of hot rolling are further preferably in the ranges, the reduction is matched with the temperature, iron and silicon elements in the 6061 aluminum alloy are fully dispersed, and strip-shaped iron-rich phases (AlFeSi phases) of aluminum, iron and silicon are avoided.
Preferably, the temperature of the solution treatment in the step (5) is 500 to 530 ℃, and may be, for example, 500 ℃, 504 ℃, 507 ℃, 510 ℃, 514 ℃, 517 ℃, 520 ℃, 524 ℃, 527 ℃, or 530 ℃, but is not limited to the recited values, and other values not recited in the range are also applicable.
Preferably, the time of the solution treatment in the step (5) is 2 to 8 hours, for example, 2 hours, 2.7 hours, 3.4 hours, 4 hours, 4.7 hours, 5.4 hours, 6 hours, 6.7 hours, 7.4 hours or 8 hours, etc., but not limited to the enumerated values, and other values not enumerated within the range are also applicable.
Preferably, the cooling after the solution treatment in the step (5) is water cooling.
Preferably, the cold rolling in step (5) is performed at a reduction amount of 0.5 to 5%, for example, 0.5%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, or 5%, but not limited to the above-mentioned values, and other values not listed in this range are also applicable.
The method particularly needs to strictly control the pressing amount of cold rolling within the range, can control the material to be pressed at 15-40 ℃ at one time, realizes the refinement of crystal grains in the material, enables the residual slightly strip-shaped AlFeSi phase to be crushed, achieves the effect of converting the AlFeSi phase into particles through subsequent aging treatment, and greatly improves the corrosion resistance of the material.
Preferably, the temperature of the aging treatment in the step (6) is 130 to 250 ℃, and may be, for example, 130 ℃, 140 ℃, 150 ℃, 170 ℃, 180 ℃, 190 ℃, 210 ℃, 220 ℃, 230 ℃, or 250 ℃, but is not limited to the recited values, and other values not recited in the range are also applicable.
Preferably, the heat preservation time of the aging treatment in the step (6) is 1 to 24 hours, for example, 1 hour, 4 hours, 7 hours, 9 hours, 12 hours, 14 hours, 17 hours, 19 hours, 22 hours or 24 hours, etc., but not limited to the enumerated values, and other values not enumerated in the range are also applicable.
Preferably, the cooling method in the aging treatment in the step (6) is air cooling.
As a preferred technical scheme of the invention, the method comprises the following steps:
(1) homogenizing and annealing the 6061 aluminum alloy blank at 550-580 ℃ for 12-24 h to obtain a homogenized and annealed blank;
(2) placing the homogenized and annealed blank in a heating furnace, carrying out primary preheating to 400-500 ℃, carrying out primary heat preservation for 5-30 min, and then carrying out forging for at least three times, wherein the forging ratio of single forging is 1.5-2.5, so as to obtain a forged blank;
(3) annealing the forged blank through heat treatment at 300-500 ℃, and performing water cooling after heat preservation for 60-180 min in the heat treatment annealing to obtain a blank after heat treatment annealing;
(4) placing the blank subjected to heat treatment annealing in a heating furnace, carrying out second preheating to 350-450 ℃, carrying out second heat preservation for 5-30 min, and then carrying out hot rolling, wherein the rolling deformation of the hot rolling is 30-80%, and the pressing amount of each pass is 19-21 mm, so as to obtain a hot-rolled blank;
(5) carrying out solution treatment for 2-8 h and water cooling on the hot-rolled blank at 500-530 ℃, and then carrying out cold rolling with the cold rolling reduction of 0.5-5% to obtain a cold-rolled blank;
(6) and (3) sequentially carrying out aging treatment for 1-24 h and leveling on the cold-rolled blank at 130-250 ℃ to obtain the 6061 aluminum alloy containing the granular iron-rich phase.
According to the invention, through the combination of all steps and process parameters, the ring between each step is buckled, so that the final corrosion resistance of the 6061 aluminum alloy is influenced, and the corrosion resistance of the material is influenced after the steps and the sequence are adjusted.
In a second aspect, the present invention provides a 6061 aluminum alloy containing a particulate iron-rich phase, wherein the 6061 aluminum alloy is prepared by the method for preparing the 6061 aluminum alloy containing the particulate iron-rich phase according to the first aspect.
The 6061 aluminum alloy provided by the second aspect of the invention has the iron-rich phase existing in a granular form, so that a galvanic cell is not formed in the material any more, and the material does not contain a lath-shaped iron-rich phase (AlFeSi phase), and the corrosion resistance is obviously improved.
Preferably, the 6061 aluminum alloy comprises the following components in percentage by mass: 0.4 to 0.8 percent of Si; fe is less than or equal to 0.04 percent; 0.15 to 0.25 percent of Cu; mn is less than or equal to 0.15 percent; 0.8 to 1.2 percent of Mg; 0.04 to 0.35 percent of Cr; zn is less than or equal to 0.25 percent; less than or equal to 0.15 percent of Ti, and the balance of aluminum and inevitable impurities.
In the composition of the aluminum alloy 6061 of the present invention, Si may be 0.4 to 0.8%, for example, 0.4%, 0.45%, 0.49%, 0.54%, 0.58%, 0.63%, 0.67%, 0.72%, 0.76%, or 0.8%, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Fe is 0.04% or less, and may be, for example, 0.01%, 0.02%, 0.03%, or 0.04%, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Cu is 0.15 to 0.4%, and may be, for example, 0.15%, 0.18%, 0.2%, 0.21%, 0.22%, 0.23%, 0.24%, 0.25%, 0.3%, 0.35%, 0.38%, or 0.4%, but is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned range are also applicable.
Mn is 0.15% or less, and may be, for example, 0.05%, 0.07%, 0.08%, 0.09%, 0.1%, 0.11%, 0.12%, 0.13%, 0.14%, or 0.15%, but is not limited to the values listed, and other values not listed in the range are also applicable.
0.8 to 1.2% of Mg may be, for example, 0.8%, 0.85%, 0.89%, 0.94%, 0.98%, 1.03%, 1.07%, 1.12%, 1.16%, or 1.2%, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
0.04 to 0.35% of Cr, for example, 0.04%, 0.08%, 0.11%, 0.15%, 0.18%, 0.22%, 0.25%, 0.29%, 0.32%, or 0.35%, etc., but not limited to the above-mentioned values, and other values not listed in the above range are also applicable.
Zn is 0.25% or less, and may be, for example, 0.1%, 0.2%, 0.3%, or 0.25%, but not limited to the values listed, and other values not listed in the range are also applicable.
Ti is 0.15% or less, and may be, for example, 0.05%, 0.07%, 0.08%, 0.09%, 0.1%, 0.11%, 0.12%, 0.13%, 0.14%, or 0.15%, but is not limited to the values listed, and other values not listed in the range are also applicable.
In a third aspect, the present invention provides a gas distribution plate made of the 6061 aluminum alloy containing a particulate iron-rich phase according to the second aspect.
The gas distribution plate of the third aspect of the invention adopts the 6061 aluminum alloy with high corrosion resistance, so that the service life is long and the application effect is good.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) the preparation method of the 6061 aluminum alloy containing the granular iron-rich phase provided by the invention does not need to change the component proportion of the 6061 aluminum alloy, can realize the optimization of performance by adopting the conventionally purchased 6061 blank only through a manufacturing process, and has low cost and simple flow;
(2) the 6061 aluminum alloy containing the granular iron-rich phase provided by the invention does not contain a lath-shaped AlFeSi phase in the interior, the unidirectional maximum size of the granular AlFeSi phase can be controlled within 36 mu m, the unidirectional maximum size of the general granules can be controlled within 20 mu m, the unidirectional maximum size of the granular AlFeSi phase can be controlled within 20 mu m under the optimal condition, a galvanic cell is not formed any more, and the corrosion resistance is obviously improved;
(3) the corrosion resistance of the 6061 aluminum alloy adopted by the gas distribution plate provided by the invention is remarkably improved, the traditional 6061 aluminum alloy only resists a 5% NaOH solution for 30s, the 6061 aluminum alloy provided by the invention can resist the 5% NaOH solution for more than 5min, a ceramic layer or an anti-corrosion layer does not need to be coated on the outer side, the risk of peeling of the anti-corrosion layer is avoided, the product is integrally formed, the gas distribution plate is simple and easy to manufacture, and the industrial application prospect is wide.
Drawings
FIG. 1 is an SEM image of 6061 aluminum alloy made according to example 1 of the invention.
Fig. 2 is a partially enlarged view of fig. 1.
FIG. 3 is an SEM image of 6061 aluminum alloy from inventive example 5.
FIG. 4 is an SEM image of 6061 aluminum alloy from inventive example 6.
FIG. 5 is an SEM image of 6061 aluminum alloy of example 11 of the invention.
FIG. 6 is an SEM image of 6061 aluminum alloy of comparative example 4 of the present invention.
FIG. 7 is an SEM image of 6061 aluminum alloy of comparative example 5 of the invention.
Fig. 8 is a partially enlarged view of fig. 7.
FIG. 9 is an SEM image of 6061 aluminum alloy of comparative example 6 of the present invention.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the appended claims.
Example 1
The embodiment provides a preparation method of a 6061 aluminum alloy containing a granular iron-rich phase, which comprises the following steps:
(1) homogenizing and annealing 6061 aluminum alloy blank (0.5% of Si, 0.02% of Fe, 0.18% of Cu, 0.10% of Mn, 1.0% of Mg, 0.25% of Cr, 0.20% of Zn, 0.10% of Ti and the balance of aluminum and inevitable impurities) at 570 ℃ for 18h to obtain homogenized and annealed blank;
(2) placing the homogenized and annealed blank in a heating furnace, carrying out first preheating to 450 ℃, carrying out first heat preservation for 25min, taking out the blank from the heating furnace, and carrying out three times of forging, wherein the forging ratio of each time of forging is 2.0, so as to obtain a forged blank;
(3) annealing the forged blank through heat treatment at 350 ℃, and performing water cooling after heat preservation for 120min in the heat treatment annealing to obtain a blank after heat treatment annealing;
(4) placing the blank subjected to heat treatment annealing in a heating furnace, carrying out second preheating to 380 ℃, carrying out second heat preservation for 25min, taking out the blank from the heating furnace, and carrying out hot rolling, wherein the rolling deformation of the hot rolling is 60%, and the pressing amount of each pass is 20mm, so as to obtain a hot-rolled blank;
(5) carrying out solution treatment for 7h at 520 ℃ and water cooling to 25 ℃ in sequence on the hot rolled blank, and then carrying out cold rolling with the cold rolling reduction of 3.5% to obtain a cold rolled blank;
(6) and (3) sequentially carrying out aging treatment for 12h and leveling on the cold-rolled blank at 200 ℃ to obtain the 6061 aluminum alloy containing the granular iron-rich phase.
The SEM images of the 6061 aluminum alloy prepared by the embodiment are shown in figures 1-2, and as can be seen from the images, a lath-shaped continuous iron-rich phase (white particles) does not exist any more, but exists in a granular form, wherein the unidirectional maximum size of the particles is only 18 microns, the maximum size of the particles is generally less than 15 microns, and the average particle size is less than 10 microns. And a corrosion resistance experiment is carried out by adopting a 5% sodium hydroxide solution, and the corrosion resistance is found to be more than 6 min.
Example 2
This example provides a process for producing a 6061 aluminum alloy containing a particulate iron-rich phase, which is the same as that of example 1 except that the temperature of the homogenizing annealing in step (1) is 600 ℃.
Example 3
This example provides a process for producing a 6061 aluminum alloy containing a particulate iron-rich phase, which is the same as that of example 1 except that the temperature of the homogenizing annealing in step (1) is 520 ℃.
Example 4
This example provides a process for producing a 6061 aluminum alloy containing a particulate iron-rich phase, which is the same as that of example 1 except that the temperature of the first preheating in step (2) is 520 ℃.
Example 5
This example provides a method of producing a 6061 aluminum alloy containing a particulate iron-rich phase, which is the same as that of example 1 except that the forging ratio per forging in step (2) is 3.0.
The SEM image of the 6061 aluminum alloy produced in this example is shown in FIG. 3, from which it can be seen that the lath-like continuous iron-rich phase (white particles) is no longer present, but is present in the form of particles, but the particles have a larger maximum unidirectional dimension than that of example 1, the maximum unidirectional dimension is 36 μm, the maximum unidirectional dimension of the particles is typically less than 30 μm, and the average particle size is less than 13 μm.
Example 6
This example provides a method of producing a 6061 aluminum alloy containing a particulate iron-rich phase, which is the same as that of example 1 except that the forging ratio per forging in step (2) is 1.2.
The SEM image of the 6061 aluminum alloy prepared in this example is shown in FIG. 4, and it can be seen from the image that the lath-shaped continuous iron-rich phase (white particles) is not existed any more, but exists in the form of particles, the particles are fine, but more and concentrated, the unidirectional maximum size is only 20 μm, the maximum size of the general particles is less than 9 μm, and the average particle size is less than 6 μm.
Example 7
This example provides a process for producing a 6061 aluminum alloy containing a particulate iron-rich phase, which is the same as that of example 1 except that the temperature of the heat treatment annealing in step (3) is 520 ℃.
Example 8
This example provides a process for producing a 6061 aluminum alloy containing a particulate iron-rich phase, which is the same as that of example 1 except that the temperature of the heat treatment annealing in step (3) is 280 ℃.
Example 9
This example provides a process for producing a 6061 aluminum alloy containing a particulate iron-rich phase, which is the same as that of example 1 except that the reduction per pass in step (4) is 23 mm.
Example 10
This example provides a process for producing a 6061 aluminum alloy containing a particulate iron-rich phase, which is the same as in example 1 except that the reduction amount in the cold rolling in step (5) is 6%.
Example 11
This example provides a process for producing a 6061 aluminum alloy containing a particulate iron-rich phase, which is the same as in example 1 except that the reduction amount in the cold rolling in step (5) is 0.4%.
The SEM image of the 6061 aluminum alloy prepared in this example is shown in FIG. 5, and it can be seen from the image that the lath-like continuous iron-rich phase (white particles) is no longer present, but exists in the form of particles, but the unidirectional maximum size is larger than that of example 1, the unidirectional maximum size of the particles is 27 μm, the unidirectional maximum size of the general particles is less than 16 μm, and the average particle size is less than 14 μm. And a corrosion resistance experiment is carried out by adopting a 5% sodium hydroxide solution, and the corrosion resistance is found to be more than 5 min.
Example 12
This example provides a process for producing a 6061 aluminum alloy containing a particulate iron-rich phase, which is the same as that of example 1 except that the temperature of the aging treatment in step (5) is 270 ℃.
Example 13
This example provides a process for producing a 6061 aluminum alloy containing a particulate iron-rich phase, which is the same as that of example 1 except that the temperature of the aging treatment in step (5) is 110 ℃.
Example 14
This example provides a method for preparing a 6061 aluminum alloy containing a particulate iron-rich phase, comprising the steps of:
(1) a 6061 aluminum alloy blank (0.4 percent of Si, 0.03 percent of Fe, 0.25 percent of Cu, 0.50 percent of Mn, 1.2 percent of Mg, 0.04 percent of Cr, 0.25 percent of Zn, 0.15 percent of Ti, and the balance of aluminum and inevitable impurities) is subjected to homogenization annealing at 580 ℃ for 12 hours to obtain a homogenized and annealed blank;
(2) placing the homogenized and annealed blank in a heating furnace, carrying out first preheating to 500 ℃, carrying out first heat preservation for 5min, taking out the blank from the heating furnace, and carrying out three-time forging, wherein the forging ratio of each forging is 2.5, so as to obtain a forged blank;
(3) annealing the forged blank by heat treatment at 500 ℃, and performing water cooling after keeping the temperature for 180min in the heat treatment annealing to obtain a blank after the heat treatment annealing;
(4) placing the blank subjected to heat treatment annealing in a heating furnace, carrying out second preheating to 350 ℃, carrying out second heat preservation for 30min, taking out the blank from the heating furnace, and carrying out hot rolling, wherein the rolling deformation of the hot rolling is 80%, and the pressing amount of each pass is 19mm, so as to obtain a hot-rolled blank;
(5) carrying out solution treatment on the hot-rolled blank at 530 ℃ for 2h and water cooling to 20 ℃, and then carrying out cold rolling with the cold rolling reduction of 5% to obtain a cold-rolled blank;
(6) and (3) sequentially carrying out aging treatment for 1h and leveling on the cold-rolled blank at 250 ℃ to obtain the 6061 aluminum alloy containing the granular iron-rich phase.
And a corrosion resistance experiment is carried out by adopting a 5% sodium hydroxide solution, and the corrosion resistance is found to be more than 7 min.
Example 15
This example provides a method for preparing a 6061 aluminum alloy containing a particulate iron-rich phase, comprising the steps of:
(1) homogenizing and annealing 6061 aluminum alloy blank (0.8% of Si, 0.04% of Fe, 0.17% of Cu, 0.10% of Mn, 0.9% of Mg, 0.1% of Cr, 0.20% of Zn, 0.10% of Ti and the balance of aluminum and inevitable impurities) at 550 ℃ for 20 hours to obtain homogenized and annealed blank;
(2) placing the homogenized and annealed blank in a heating furnace, preheating to 480 ℃ for the first time, keeping the temperature for 15min for the first time, taking out the blank from the heating furnace, and forging for three times, wherein the forging ratio of each forging is 1.5, so as to obtain a forged blank;
(3) annealing the forged blank through heat treatment at 400 ℃, and performing water cooling after heat preservation for 100min in the heat treatment annealing to obtain a blank after heat treatment annealing;
(4) placing the blank subjected to heat treatment annealing in a heating furnace, carrying out second preheating to 400 ℃, carrying out second heat preservation for 20min, taking out the blank from the heating furnace, and carrying out hot rolling, wherein the rolling deformation of the hot rolling is 45%, and the pressing amount of each pass is 21mm, so as to obtain a hot-rolled blank;
(5) carrying out solution treatment for 4h at 510 ℃ and water cooling to 35 ℃ in sequence on the hot rolled blank, and then carrying out cold rolling with the pressing amount of the cold rolling being 1.5% to obtain a cold rolled blank;
(6) and (3) sequentially carrying out aging treatment for 20h and leveling on the cold-rolled blank at 150 ℃ to obtain the 6061 aluminum alloy containing the granular iron-rich phase.
And (3) performing corrosion resistance experiments by using a 5% sodium hydroxide solution, and finding that the corrosion resistance can be improved by more than 9 min.
Comparative example 1
This comparative example provides a 6061 aluminum alloy production method which is the same as that of example 1 except that the forging in step (2) is not performed. The corrosion resistance experiment is carried out by using a 5% sodium hydroxide solution, and the corrosion resistance is only 25s, namely, the corrosion condition is found.
Comparative example 2
This comparative example provides a process for producing a 6061 aluminum alloy, which is the same as in example 1 except that the homogenization annealing in step (1) is not performed. The corrosion resistance experiment is carried out by using a 5% sodium hydroxide solution, and the corrosion resistance is only 30s, namely, the corrosion condition is found.
Comparative example 3
This comparative example provides a 6061 aluminum alloy production method which is the same as that of example 1 except that the heat treatment annealing in step (3) is not performed. The corrosion resistance experiment is carried out by using a 5% sodium hydroxide solution, and the corrosion resistance is only 35s, namely, the corrosion condition is found.
Comparative example 4
This comparative example provides a production method of 6061 aluminum alloy, which is the same as example 1 except that the cold rolling in step (6) is not performed.
The SEM image of the 6061 aluminum alloy obtained in this comparative example is shown in fig. 6, and it can be seen from fig. 6 that the iron-rich phase is in the form of a lath, the longest dimension of each of the lath-shaped iron-rich phases is 120 μm or more, and the length thereof is about 35 μm or more, and they are connected to each other to form a mesh, which makes it easy to construct a galvanic cell. The corrosion resistance experiment is carried out by using a 5% sodium hydroxide solution, and the corrosion resistance is only 25s, namely, the corrosion condition is found.
Comparative example 5
This comparative example provides a 6061 aluminum alloy production method which is the same as example 1 except that the cold rolling + aging treatment of step (6) is performed first, and the hot rolling + solution treatment of steps (4) and (5) is performed.
The method comprises the following specific steps:
(4) cold rolling the blank after the heat treatment annealing, wherein the pressing amount of the cold rolling is 3.5 percent to obtain a cold-rolled blank, and the cold-rolled blank is subjected to aging treatment for 12 hours at 200 ℃;
(5) placing the aged blank in a heating furnace, carrying out second preheating to 380 ℃, carrying out second heat preservation for 25min, taking out the blank from the heating furnace, and carrying out hot rolling, wherein the rolling deformation of the hot rolling is 60%, and the pressing amount of each pass is 20mm, so as to obtain a hot-rolled blank;
(6) and (3) carrying out solution treatment for 7h at 520 ℃ and water cooling on the hot-rolled blank in sequence, and leveling to obtain the 6061 aluminum alloy containing the granular iron-rich phase.
SEM images of the 6061 aluminum alloy prepared by the comparative example are shown in FIGS. 7 to 8, and it can be seen from FIGS. 7 to 8 that the iron-rich phase is in the form of lath, the longest dimension of each strip of the iron-rich phase can reach more than 90 μm, and the length of each strip of the iron-rich phase is about more than 40 μm, and the iron-rich phase and the strip of the iron-rich phase are mutually connected to form a net, so that a galvanic cell is easily formed. The corrosion resistance experiment is carried out by using a 5% sodium hydroxide solution, and the corrosion resistance is only 30s, namely, the corrosion condition is found.
Comparative example 6
This comparative example provides a 6061 aluminum alloy production method similar to example 1, except that the hot rolling of step (4) and the solution treatment of step (5) are performed first, and the forging of step (2) and the heat treatment annealing of step (3) are performed.
The method comprises the following specific steps:
(1) homogenizing and annealing 6061 aluminum alloy blank (0.5% of Si, 0.02% of Fe, 0.18% of Cu, 0.10% of Mn, 1.0% of Mg, 0.25% of Cr, 0.20% of Zn, 0.10% of Ti and the balance of aluminum and inevitable impurities) at 570 ℃ for 18h to obtain homogenized and annealed blank;
(2) placing the homogenized and annealed blank in a heating furnace, carrying out second preheating to 380 ℃, carrying out second heat preservation for 25min, taking out the blank from the heating furnace, and carrying out hot rolling, wherein the rolling deformation of the hot rolling is 60%, and the pressing amount of each pass is 20mm, so as to obtain a hot-rolled blank;
(3) the hot-rolled blank is subjected to solution treatment for 7 hours at 520 ℃ and water cooling in sequence, then is placed in a heating furnace, is subjected to first preheating to 450 ℃ and is subjected to first heat preservation for 25min, and then is taken out of the heating furnace for three times of forging, wherein the forging ratio of each forging is 2.0, so that a forged blank is obtained;
(4) annealing the forged blank through heat treatment at 350 ℃, keeping the temperature for 120min, and then cooling by water to obtain a blank after heat treatment and annealing;
(5) cold rolling the blank after the heat treatment annealing, wherein the pressing amount of the cold rolling is 3.5 percent, and obtaining the cold-rolled blank;
(6) and (3) sequentially carrying out aging treatment for 12h and leveling on the cold-rolled blank at 200 ℃ to obtain the 6061 aluminum alloy containing the granular iron-rich phase.
The SEM image of the 6061 aluminum alloy obtained in this comparative example is shown in fig. 9, and it can be seen from fig. 9 that the iron-rich phase is in the form of a lath, the longest dimension of each of the lath-shaped iron-rich phases is up to 75 μm or more, and the length thereof is about 32 μm or more, and they are connected with each other to form a mesh, which makes it easy to construct a galvanic cell. The corrosion resistance experiment is carried out by using a 5% sodium hydroxide solution, and the corrosion resistance is only 30s, namely, the corrosion condition is found.
The test method comprises the following steps: the surface of the obtained 6061 aluminum alloy is characterized by adopting SEM, whether a lath-shaped AlFeSi phase is formed in the surface is inspected, and the size of the lath-shaped or granular AlFeSi phase is measured and evaluated.
The test results of the above examples and comparative examples are shown in table 1.
TABLE 1
From table 1, the following points can be seen:
(1) it can be seen from the comprehensive examples 1 to 15 that the preparation method of the 6061 aluminum alloy containing the granular iron-rich phase provided by the invention can convert the lath-shaped iron-rich phase in the 6061 aluminum alloy system into granules, thereby avoiding the formation of a galvanic cell and improving the corrosion resistance, wherein the unidirectional maximum size of the AlFeSi phase in all the granules can be controlled within 36 μm, and the unidirectional maximum size of the general granules can be controlled within 20 μm;
(2) it can be seen from the comprehensive examples 1 and comparative examples 5 to 6 that the sequence among the steps in the invention is very critical, the example 1 is strictly carried out according to the sequence of homogenizing annealing, first preheating, forging, heat treatment annealing, second preheating, hot rolling, solution treatment, cold rolling and aging treatment, compared with the operation sequence adjusted in the comparative examples 5 to 6, the iron-rich phase in the final product in the example 1 is granular, and the iron-rich phase in the comparative examples 5 to 6 is strip-shaped, so that the galvanic cell is easily formed, thereby showing that the steps are buckled with each other in a ring-to-ring manner, the structure of the product is improved by strictly controlling the sequence relationship, and the corrosion resistance of the 6061 aluminum alloy is improved;
(3) it can be seen from the combination of example 1 and comparative examples 1 to 4 that each step is not necessary, when a certain step is not available, a granular iron-rich phase is difficult to form, the unidirectional size of the batten can reach more than 100 microns at most, the local corrosion is serious, and the service life of the material is remarkably reduced.
The present invention is described in detail with reference to the above embodiments, but the present invention is not limited to the above detailed structural features, that is, the present invention is not meant to be implemented only by relying on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (10)
1. A method for preparing 6061 aluminum alloy containing granular iron-rich phase is characterized by comprising the following steps:
(1) carrying out homogenization annealing on the 6061 aluminum alloy blank to obtain a homogenized and annealed blank;
(2) forging the homogenized and annealed blank for at least three times after first preheating and first heat preservation to obtain a forged blank;
(3) carrying out heat treatment annealing on the forged blank to obtain a heat-treated and annealed blank;
(4) secondly preheating the blank subjected to the heat treatment annealing, carrying out second heat preservation, and then carrying out hot rolling to obtain a hot-rolled blank;
(5) the hot-rolled blank is subjected to solution treatment and cooling in sequence, and then is subjected to cold rolling to obtain a cold-rolled blank;
(6) and (3) sequentially carrying out aging treatment and leveling on the cold-rolled blank to obtain the 6061 aluminum alloy containing granular iron-rich phase.
2. The preparation method according to claim 1, wherein the temperature of the homogenizing annealing in the step (1) is 550 to 580 ℃;
preferably, the time of the homogenizing annealing in the step (1) is 12-24 h.
3. The method according to claim 1 or 2, wherein the temperature of the first preheating in the step (2) is 400 to 500 ℃;
preferably, the first heat preservation time in the step (2) is 5-30 min;
preferably, the first preheating in step (2) is performed in a heating furnace;
preferably, the forging ratio of the forging in the step (2) is 1.5-2.5.
4. The method according to any one of claims 1 to 3, wherein the temperature of the heat treatment annealing in the step (3) is 300 to 500 ℃;
preferably, the heat preservation time of the heat treatment annealing in the step (3) is 60-180 min;
preferably, the cooling manner after the heat preservation in the heat treatment annealing in the step (3) includes water cooling.
5. The method according to any one of claims 1 to 4, wherein the temperature of the second preheating in the step (4) is 350 to 450 ℃;
preferably, the second heat preservation time in the step (4) is 5-30 min;
preferably, the second preheating in step (4) is performed in a heating furnace;
preferably, the rolling deformation amount of the hot rolling in the step (4) is 30-80%;
preferably, the reduction amount of each pass of the hot rolling in the step (4) is 19-21 mm.
6. The method according to any one of claims 1 to 5, wherein the temperature of the solution treatment in the step (5) is 500 to 530 ℃;
preferably, the time of the solution treatment in the step (5) is 2-8 h;
preferably, the cooling after the solution treatment in the step (5) is water cooling;
preferably, the amount of cold rolling in step (5) is 0.5 to 5%.
7. The method according to any one of claims 1 to 6, wherein the temperature of the aging treatment in the step (6) is 130 to 250 ℃;
preferably, the heat preservation time of the aging treatment in the step (6) is 1-24 h;
preferably, the cooling method in the aging treatment in the step (6) is air cooling.
8. The method for preparing a composite material according to any one of claims 1 to 7, wherein the method comprises the steps of:
(1) homogenizing and annealing the 6061 aluminum alloy blank at 550-580 ℃ for 12-24 h to obtain a homogenized and annealed blank;
(2) placing the homogenized and annealed blank in a heating furnace, carrying out primary preheating to 400-500 ℃, carrying out primary heat preservation for 5-30 min, and then carrying out forging for at least three times, wherein the forging ratio of single forging is 1.5-2.5, so as to obtain a forged blank;
(3) annealing the forged blank through heat treatment at 300-500 ℃, and performing water cooling after heat preservation for 60-180 min in the heat treatment annealing to obtain a blank after heat treatment annealing;
(4) placing the blank subjected to heat treatment and annealing in a heating furnace, carrying out second preheating to 350-450 ℃, carrying out second heat preservation for 5-30 min, and then carrying out hot rolling, wherein the rolling deformation of the hot rolling is 30-80%, and the pressing amount of each pass is 19-21 mm, so as to obtain a hot-rolled blank;
(5) carrying out solution treatment on the hot-rolled blank at 500-530 ℃ for 2-8 h, cooling with water, and then carrying out cold rolling, wherein the cold rolling reduction is 0.5-5%, so as to obtain a cold-rolled blank;
(6) and (3) sequentially carrying out aging treatment for 1-24 h and leveling on the cold-rolled blank at 130-250 ℃ to obtain the 6061 aluminum alloy containing the granular iron-rich phase.
9. A 6061 aluminum alloy containing a granular iron-rich phase, wherein the 6061 aluminum alloy is prepared by the preparation method of the 6061 aluminum alloy containing the granular iron-rich phase according to any one of claims 1 to 8.
10. A gas distribution plate made of the 6061 aluminum alloy containing the granular iron-rich phase according to claim 9.
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| CN102644039A (en) * | 2011-02-17 | 2012-08-22 | 北京有色金属研究总院 | Preparation method of high-quality 6061 aluminium alloy forging for semiconductor equipment |
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