An aluminum alloy forging for a gas distribution plate of a semiconductor device and a manufacturing method thereof

Abstract

The application discloses a kind of aluminium alloy forgings of uniform air disc for semiconductor equipment and preparation process, it is related to aluminium alloy forging technical field, the preparation process includes: Al 6061 aluminium alloy bar is carried out grading homogenization treatment;Adopt three-stage free forging forming;After T652 heat treatment, obtain the uniform air disc base with compact structure, high-temperature strength is promoted;High-entropy alloy support bottom layer and yttrium oxide surface layer are sequentially deposited using plasma spraying, support bottom layer raw material is AlCoCrFeNi high-entropy alloy powder after twice plasma spraying-quenching cycle pretreatment, uniformly distributed in-situ generated nanometer alumina dispersion phase, surface layer raw material is yttrium oxide powder.The application realizes coating and base strong combination, anti-plasma corrosion, prevent particle shedding and the synergistic promotion of thermal dimensional stability by base structure optimization and gradient coating design, meet the stringent requirements of semiconductor etching equipment on uniform air disc long service life, high cleanliness.

Description

Technical Field

[0001] This invention relates to the field of aluminum alloy forging technology, specifically to an aluminum alloy forging for a gas distribution plate for semiconductor equipment and its manufacturing process. Background Technology

[0002] Gas leveling disks in semiconductor etching equipment are key components determining process uniformity and wafer yield. They are typically made of Al6061 aluminum alloy through forging and heat treatment. As etching processes evolve towards high-power, high-density plasma, gas leveling disks face increasingly demanding operating conditions. Existing technologies suffer from the following main shortcomings:

[0003] Although Al 6061 aluminum alloy has good machinability, traditional forging and heat treatment processes cannot completely eliminate casting segregation and internal micropore defects, resulting in limited microstructure uniformity. Under the repeated thermal cycling of the etching process, the residual stress distribution inside the substrate is uneven, which easily leads to local plastic deformation, resulting in deterioration of the flatness of the gas distribution disk, affecting the uniformity of the gas flow field distribution, and thus reducing the stability of the etching process.

[0004] Existing surface treatments for gas distribution disks mostly employ anodizing or traditional ceramic coatings. However, in highly corrosive plasma environments containing fluorine, chlorine, etc., the anodized layer is easily eroded, resulting in increased surface roughness and the introduction of particulate contamination sources. Traditional ceramic coatings (such as alumina and zirconium oxide) are prone to phase transitions or microcrack propagation under long-term plasma bombardment, leading to a decrease in coating integrity and making it difficult to meet the requirements of advanced processes in terms of protection life.

[0005] The difference in thermal expansion coefficients between the aluminum alloy substrate and the ceramic coating makes it easy for thermal stress to accumulate at the interface during thermal cycling. Existing coating systems lack effective stress buffer layer designs, and the interface bonding is mainly based on mechanical anchoring, which has limited bonding strength. Under temperature fluctuations or plasma impacts, localized coating peeling is prone to occur, and the peeling particles cause cross-contamination of the wafer, seriously affecting product yield.

[0006] Semiconductor processes require extremely stringent control over particulate contamination within the cavity. During long-term service, existing gas distribution disk surface treatment layers experience the shedding of micron-sized particles due to corrosion, phase transitions, or interface failures, becoming a significant source of contamination. Traditional surface treatment technologies struggle to balance corrosion resistance with low particle release characteristics, hindering the extension of equipment maintenance cycles and the improvement of process yield.

[0007] In summary, existing Al 6061 aluminum alloy gas distribution disks have significant shortcomings in terms of substrate microstructure stability, surface corrosion resistance, coating interface bonding strength, and particle control. There is an urgent need to develop a gas distribution disk preparation technology that combines a high-strength and tough substrate, a strong-bonding coating, and a plasma-resistant surface layer to meet the stringent requirements of advanced semiconductor processes for long component life, high cleanliness, and dimensional stability. Summary of the Invention

[0008] The purpose of this invention is to provide an aluminum alloy forging for a gas distribution disk for semiconductor devices and its manufacturing process, so as to solve the problems raised in the prior art.

[0009] To achieve the above objectives, the present invention provides the following technical solution:

[0010] A manufacturing process for an aluminum alloy forging for a gas distribution disk for semiconductor devices includes the following steps:

[0011] S1: Graded homogenization treatment: Using Al 6061 aluminum alloy bars as raw materials, first heat them at 450-455℃ for 5-5.5h, then heat them to 550-555℃ for 24h to obtain homogenized bars.

[0012] S2: Three-stage free forging: First, a ceramic fiber pad is laid on the hydraulic press worktable for upsetting; then, a V-shaped anvil forging control flow line is used for drawing; the die is preheated to 250-255℃ for die finishing to obtain the forging billet;

[0013] S3: T652 heat treatment: The forged billet is subjected to solution treatment, water quenching, cold pressing, artificial aging, and air cooling to room temperature in sequence to obtain the uniform gas disk aluminum alloy forging base;

[0014] S4: Plasma spraying: Plasma spraying is used to deposit a high-entropy alloy support bottom layer and a yttrium oxide surface layer on the surface of the gas distribution plate aluminum alloy forging substrate, and air-cooled to room temperature to obtain the gas distribution plate aluminum alloy forging for semiconductor equipment.

[0015] Furthermore, during the plasma spraying process, the substrate temperature is stabilized at 150-180℃ by air cooling;

[0016] Furthermore, the air-cooling cooling rate is ≤5℃ / min;

[0017] Furthermore, the high-entropy alloy support substrate material is pretreated AlCoCrFeNi high-entropy alloy powder obtained through two plasma spraying-quenching cycles, with a particle size of 15-20 μm; the yttrium oxide surface material is yttrium oxide powder with a particle size of 15-45 μm.

[0018] Furthermore, the preparation method of the pretreated AlCoCrFeNi high-entropy alloy powder includes the following steps: Step 1: Dry the AlCoCrFeNi high-entropy alloy powder in an argon atmosphere at 150-155℃ for 30-45 minutes to obtain powder A;

[0019] Step 2: Spray powder A into distilled water coolant, collect the deposited powder, filter, ultrasonically clean, dry, and sieve. Repeat the above steps once to obtain pretreated AlCoCrFeNi high-entropy alloy powder.

[0020] Furthermore, in the preparation process of the pretreated AlCoCrFeNi high-entropy alloy powder, the spraying parameters are: power 32-34kW, voltage 60V, current 520A, spray gun distance 180-200mm, powder feeding rate 4-4.2L / min, argon flow rate 0-40L / min, and hydrogen flow rate 30-32L / min.

[0021] Furthermore, in the preparation process of the aluminum alloy forging for the gas distribution plate for semiconductor equipment, the plasma spraying parameters for the high-entropy alloy support underlayer are: power 80-90kW, argon flow rate 180-220L / min, hydrogen flow rate 40-60L / min, powder feeding rate 45-60g / min, and spraying distance 100-120mm.

[0022] Furthermore, in the preparation process of the aluminum alloy forging for the gas distribution plate for semiconductor equipment, the plasma spraying parameters for the yttrium oxide surface layer are as follows: power 65-75kW, argon flow rate 160-200L / min, hydrogen flow rate 30-50L / min, powder feeding rate 35-50g / min, and spraying distance 90-110mm.

[0023] Furthermore, the thickness of the supporting substrate is 20-30 μm, the thickness of the yttrium oxide surface layer is 5-10 μm, and the total coating thickness is 25-40 μm.

[0024] Furthermore, during the upsetting process, the forging temperature is 415-425℃, the total reduction is 35%, the forging speed is 28-32mm / s, and the single-pass reduction is ≤15%.

[0025] Furthermore, during the drawing process, the forging temperature is 375-385℃, the single-pass pressing and turning angle is 90°, the feed ratio is 0.7, and the forging temperature difference is controlled to be ≤15℃ to ensure that the metal flow lines are evenly distributed radially.

[0026] Furthermore, during the finishing process of the mold, a special fan-shaped mold with a precision of 0.1° is used to form the air hole distribution area, the temperature is 345-355℃, the pressure is 48-50MPa, and the pressure holding time is 14-16s.

[0027] Furthermore, the solution treatment parameters are: temperature 475-480℃, time 2.5-3h; the quenching parameters are: temperature 62-68℃, transfer time ≤8s; the cold pressing parameters are: applying 1.8-2.2% permanent deformation perpendicular to the main direction of the free forging streamline at room temperature, at a rate of 0.5-0.55mm / s; and the artificial aging parameters are: temperature 120-125℃, time 24h.

[0028] Furthermore, the Al 6061 aluminum alloy bar has a diameter of Φ610mm;

[0029] Furthermore, the aluminum alloy forging parameters for the gas distribution disc of the semiconductor device are a diameter of Φ150-400mm.

[0030] Compared with the prior art, the beneficial effects of the present invention are:

[0031] 1. This invention addresses the problem of Al 6061 aluminum alloy substrates being prone to thermal deformation and insufficient strength in semiconductor etching environments. It employs a graded homogenization treatment to eliminate dendrite segregation, a three-stage free forging process to refine grains and close micropores, and a T652 heat treatment to introduce uniformly distributed age-strengthening phases, thereby making the substrate structure dense and improving the high-temperature yield strength. This provides a stable load-bearing foundation for the coating and effectively suppresses plastic deformation under thermal cycling.

[0032] 2. The supporting substrate of this invention uses AlCoCrFeNi high-entropy alloy powder that has undergone two plasma spraying-quenching cycles for pretreatment. The high temperature of the plasma flame causes selective oxidation of Al and Cr. The high-speed impact of the droplets breaks down the oxide shell and embeds it into the powder, generating a uniformly distributed nano-Al2O3 dispersion phase in situ. The powder remains spherical and the particle size is refined to 15μm. This high-entropy alloy supporting substrate combines the high toughness of the FCC matrix with the high-temperature pinning strengthening effect of the nano-oxide. It maintains stable hardness at 900℃, providing reliable mechanical support and stress buffer for the surface layer.

[0033] 3. The surface layer of this invention uses a Y2O3 ceramic layer that is non-phase-transformable and chemically inert, forming a gradient structure of "tough metal base layer + hard ceramic surface layer" with the high-entropy alloy support base layer. The nano-Al2O3 in the high-entropy alloy support base layer inhibits the outward diffusion of Cr and Al, forming a double barrier, while the surface Y2O3 directly blocks the plasma corrosion medium. During the spraying process, the substrate temperature is kept stable at 150-180℃, and the slow cooling process controls the cooling rate to ≤5℃ / min. The thin-layer design matches the difference in thermal expansion coefficients, synergistically achieving resistance to plasma corrosion, prevention of particle shedding, and thermal dimensional stability, meeting the stringent service requirements of the gas distribution plate of semiconductor equipment. Detailed Implementation

[0034] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0035] The raw materials used in the following examples are all commercially available.

[0036] The preparation method of pretreated AlCoCrFeNi high-entropy alloy powder includes the following steps: Step 1: Dry AlCoCrFeNi high-entropy alloy powder in an argon atmosphere at 150℃ for 30 min to obtain powder A;

[0037] Step 2: Powder A is sprayed into distilled water coolant using a plasma spraying device. The spraying parameters are: power 32kW, voltage 60V, current 520A, spray gun distance 200mm, powder feed rate 4L / min, argon flow rate 28L / min, and hydrogen flow rate 30L / min. The deposited powder is collected, filtered, ultrasonically cleaned, dried, and sieved. The above steps are repeated once to obtain pretreated AlCoCrFeNi high-entropy alloy powder.

[0038] Example 1: A process for preparing an aluminum alloy forging for a gas equalization disk for semiconductor equipment, comprising the following steps: S1: graded homogenization treatment: using Al 6061 aluminum alloy bar as raw material, first heat it at 450℃ for 5 hours, then heat it to 550℃ and heat it for 24 hours to obtain a homogenized bar.

[0039] S2: Three-stage free forging: First, a ceramic fiber pad is laid on the hydraulic press worktable for upsetting. During upsetting, the forging temperature is 420℃, the total down pressure is 35%, the forging speed is 30mm / s, and the down pressure per pass is ≤15%. Next, a V-shaped anvil is used to control the flow lines for drawing. During drawing, the forging temperature is 380℃, the down pressure flip angle is 90°, the feed ratio is 0.7, and the forging temperature difference is controlled to ≤15℃ to ensure that the metal flow lines are radially and uniformly distributed. The die is preheated to 250℃ for die finishing. During die finishing, a special fan-shaped die with a precision of 0.1° is used to form the pore distribution area. The temperature is 350℃, the pressure is 50MPa, and the holding time is 15s to obtain the forged billet.

[0040] S3: T652 heat treatment: The forged billet is subjected to solution treatment, water quenching, cold pressing, artificial aging, and air cooling to room temperature in sequence to obtain the uniform gas disk aluminum alloy forging base;

[0041] The solution treatment parameters are: temperature 480℃, time 2.5h; the quenching parameters are: temperature 64℃, transfer time ≤8s; the cold pressing parameters are: applying 2% permanent deformation perpendicular to the main direction of the free forging streamline at room temperature, at a rate of 0.5mm / s; the artificial aging parameters are: temperature 120℃, time 24h.

[0042] S4: Plasma spraying: Plasma spraying is used to deposit a high-entropy alloy support bottom layer and a yttrium oxide surface layer on the surface of the gas distribution plate aluminum alloy forging substrate, and air-cooled to room temperature to obtain the gas distribution plate aluminum alloy forging for semiconductor equipment.

[0043] The parameters for plasma spraying of the high-entropy alloy support base layer are: power 85kW, argon flow rate 200L / min, hydrogen flow rate 50L / min, powder feeding rate 50g / min, and spraying distance 110mm.

[0044] The parameters for plasma spraying yttrium oxide surface coating are: power 70kW, argon flow rate 180L / min, hydrogen flow rate 40L / min, powder feeding rate 40g / min, and spraying distance 100mm.

[0045] The supporting bottom layer is 25 μm thick, and the yttrium oxide surface layer is 8 μm thick.

[0046] Example 2: A process for preparing an aluminum alloy forging for a gas equalization disk for semiconductor devices, comprising the following steps: S1: graded homogenization treatment: using Al 6061 aluminum alloy bar as raw material, first heat it at 450℃ for 5 hours, then heat it to 550℃ and heat it for 24 hours to obtain a homogenized bar.

[0047] S2: Three-stage free forging: First, a ceramic fiber pad is laid on the hydraulic press worktable for upsetting. During upsetting, the forging temperature is 420℃, the total down pressure is 35%, the forging speed is 30mm / s, and the down pressure per pass is ≤15%. Next, a V-shaped anvil is used to control the flow lines for drawing. During drawing, the forging temperature is 380℃, the down pressure flip angle is 90°, the feed ratio is 0.7, and the forging temperature difference is controlled to ≤15℃ to ensure that the metal flow lines are radially and uniformly distributed. The die is preheated to 250℃ for die finishing. During die finishing, a special fan-shaped die with a precision of 0.1° is used to form the pore distribution area. The temperature is 350℃, the pressure is 50MPa, and the holding time is 15s to obtain the forged billet.

[0048] S3: T652 heat treatment: The forged billet is subjected to solution treatment, water quenching, cold pressing, artificial aging, and air cooling to room temperature in sequence to obtain the uniform gas disk aluminum alloy forging base;

[0049] The solution treatment parameters are: temperature 480℃, time 2.5h; the quenching parameters are: temperature 64℃, transfer time ≤8s; the cold pressing parameters are: applying 2% permanent deformation perpendicular to the main direction of the free forging streamline at room temperature, at a rate of 0.5mm / s; the artificial aging parameters are: temperature 120℃, time 24h.

[0050] S4: Plasma spraying: Plasma spraying is used to deposit a high-entropy alloy support bottom layer and a yttrium oxide surface layer on the surface of the gas distribution plate aluminum alloy forging substrate, and air-cooled to room temperature to obtain the gas distribution plate aluminum alloy forging for semiconductor equipment.

[0051] The parameters for plasma spraying of the high-entropy alloy support base layer are: power 82kW, argon flow rate 190L / min, hydrogen flow rate 45L / min, powder feeding rate 48g / min, and spraying distance 115mm.

[0052] The parameters for plasma spraying yttrium oxide surface coating are: power 68kW, argon flow rate 170L / min, hydrogen flow rate 35L / min, powder feeding rate 38g / min, and spraying distance 105mm.

[0053] The supporting bottom layer has a thickness of 28 μm, and the yttrium oxide surface layer has a thickness of 7 μm.

[0054] Comparative Example 1: A process for preparing an aluminum alloy forging for a gas distribution disk for semiconductor equipment, comprising the following steps: on the surface of a commercially available aluminum alloy forging for a gas distribution disk substrate, a high-entropy alloy support underlayer and a yttrium oxide surface layer are sequentially deposited by plasma spraying, and then air-cooled to room temperature to obtain the aluminum alloy forging for a gas distribution disk for semiconductor equipment.

[0055] The parameters for plasma spraying of the high-entropy alloy support base layer are: power 85kW, argon flow rate 200L / min, hydrogen flow rate 50L / min, powder feeding rate 50g / min, and spraying distance 110mm.

[0056] The parameters for plasma spraying yttrium oxide surface coating are: power 70kW, argon flow rate 180L / min, hydrogen flow rate 40L / min, powder feeding rate 40g / min, and spraying distance 90-110mm.

[0057] The supporting bottom layer is 25 μm thick, and the yttrium oxide surface layer is 8 μm thick.

[0058] Comparative Example 2: A process for preparing an aluminum alloy forging for a gas equalization disk for semiconductor equipment, comprising the following steps: S1: graded homogenization treatment: using Al 6061 aluminum alloy bar as raw material, first heat it at 450℃ for 5 hours, then heat it to 550℃ and heat it for 24 hours to obtain a homogenized bar.

[0059] S2: Three-stage free forging: First, a ceramic fiber pad is laid on the hydraulic press worktable for upsetting. During upsetting, the forging temperature is 420℃, the total down pressure is 35%, the forging speed is 30mm / s, and the down pressure per pass is ≤15%. Next, a V-shaped anvil is used to control the flow lines for drawing. During drawing, the forging temperature is 380℃, the down pressure flip angle is 90°, the feed ratio is 0.7, and the forging temperature difference is controlled to ≤15℃ to ensure that the metal flow lines are radially and uniformly distributed. The die is preheated to 250℃ for die finishing. During die finishing, a special fan-shaped die with a precision of 0.1° is used to form the pore distribution area. The temperature is 350℃, the pressure is 50MPa, and the holding time is 15s to obtain the forged billet.

[0060] S3: T652 heat treatment: The forged billet is subjected to solution treatment, water quenching, cold pressing, artificial aging, and air cooling to room temperature in sequence to obtain the uniform gas disk aluminum alloy forging base;

[0061] The solution treatment parameters are: temperature 480℃, time 2.5h; the quenching parameters are: temperature 64℃, transfer time ≤8s; the cold pressing parameters are: applying 2% permanent deformation perpendicular to the main direction of the free forging streamline at room temperature, at a rate of 0.5mm / s; the artificial aging parameters are: temperature 120℃, time 24h.

[0062] S4: Plasma spraying: Plasma spraying is used to deposit a high-entropy alloy support bottom layer and a yttrium oxide surface layer on the surface of the gas distribution plate aluminum alloy forging substrate, and air-cooled to room temperature to obtain the gas distribution plate aluminum alloy forging for semiconductor equipment.

[0063] The commercially available high-entropy alloy support base layer uses commercially available AlCoCrFeNi high-entropy alloy powder without pretreatment;

[0064] The parameters for plasma spraying of the high-entropy alloy support base layer are: power 85kW, argon flow rate 200L / min, hydrogen flow rate 50L / min, powder feeding rate 50g / min, and spraying distance 110mm.

[0065] The parameters for plasma spraying yttrium oxide surface coating are: power 70kW, argon flow rate 180L / min, hydrogen flow rate 40L / min, powder feeding rate 40g / min, and spraying distance 100mm.

[0066] The supporting bottom layer is 25 μm thick, and the yttrium oxide surface layer is 8 μm thick.

[0067] Comparative Example 3: A process for preparing an aluminum alloy forging for a gas equalization disk for semiconductor equipment, comprising the following steps: S1: graded homogenization treatment: using Al 6061 aluminum alloy bar as raw material, first heat it at 450℃ for 5 hours, then heat it to 550℃ and heat it for 24 hours to obtain a homogenized bar.

[0068] S2: Three-stage free forging: First, a ceramic fiber pad is laid on the hydraulic press worktable for upsetting. During upsetting, the forging temperature is 420℃, the total down pressure is 35%, the forging speed is 30mm / s, and the down pressure per pass is ≤15%. Next, a V-shaped anvil is used to control the flow lines for drawing. During drawing, the forging temperature is 380℃, the down pressure flip angle is 90°, the feed ratio is 0.7, and the forging temperature difference is controlled to ≤15℃ to ensure that the metal flow lines are radially and uniformly distributed. The die is preheated to 250℃ for die finishing. During die finishing, a special fan-shaped die with a precision of 0.1° is used to form the pore distribution area. The temperature is 350℃, the pressure is 50MPa, and the holding time is 15s to obtain the forged billet.

[0069] S3: T652 heat treatment: The forged billet is subjected to solution treatment, water quenching, cold pressing, artificial aging, and air cooling to room temperature in sequence to obtain the uniform gas disk aluminum alloy forging base;

[0070] The solution treatment parameters are: temperature 480℃, time 2.5h; the quenching parameters are: temperature 64℃, transfer time ≤8s; the cold pressing parameters are: applying 2% permanent deformation perpendicular to the main direction of the free forging streamline at room temperature, at a rate of 0.5mm / s; the artificial aging parameters are: temperature 120℃, time 24h.

[0071] S4: Plasma spraying: A high-entropy alloy support layer is deposited on the surface of the gas distribution plate aluminum alloy forging substrate by plasma spraying, and then air-cooled to room temperature to obtain the gas distribution plate aluminum alloy forging for semiconductor equipment.

[0072] The plasma spraying parameters for the high-entropy alloy support layer are: power 85kW, argon flow rate 200L / min, hydrogen flow rate 50L / min, powder feeding rate 50g / min, and spraying distance 110mm.

[0073] The support layer is 25 μm thick.

[0074] Comparative Example 4: A process for preparing an aluminum alloy forging for a gas equalization disk for semiconductor equipment, comprising the following steps: S1: graded homogenization treatment: using Al 6061 aluminum alloy bar as raw material, first heat it at 450℃ for 5 hours, then heat it to 550℃ and heat it for 24 hours to obtain a homogenized bar.

[0075] S2: Three-stage free forging: First, a ceramic fiber pad is laid on the hydraulic press worktable for upsetting. During upsetting, the forging temperature is 420℃, the total down pressure is 35%, the forging speed is 30mm / s, and the down pressure per pass is ≤15%. Next, a V-shaped anvil is used to control the flow lines for drawing. During drawing, the forging temperature is 380℃, the down pressure flip angle is 90°, the feed ratio is 0.7, and the forging temperature difference is controlled to ≤15℃ to ensure that the metal flow lines are radially and uniformly distributed. The die is preheated to 250℃ for die finishing. During die finishing, a special fan-shaped die with a precision of 0.1° is used to form the pore distribution area. The temperature is 350℃, the pressure is 50MPa, and the holding time is 15s to obtain the forged billet.

[0076] S3: T652 heat treatment: The forged billet is subjected to solution treatment, water quenching, cold pressing, artificial aging, and air cooling to room temperature in sequence to obtain the uniform gas disk aluminum alloy forging base;

[0077] The solution treatment parameters are: temperature 480℃, time 2.5h; the quenching parameters are: temperature 64℃, transfer time ≤8s; the cold pressing parameters are: applying 2% permanent deformation perpendicular to the main direction of the free forging streamline at room temperature, at a rate of 0.5mm / s; the artificial aging parameters are: temperature 120℃, time 24h.

[0078] S4: Plasma spraying: Plasma spraying is used to deposit a yttrium oxide layer on the surface of the gas distribution plate aluminum alloy forging substrate, and air cooling is performed to room temperature to obtain the gas distribution plate aluminum alloy forging for semiconductor equipment;

[0079] The parameters for plasma spraying yttrium oxide layers are: power 70kW, argon flow rate 180L / min, hydrogen flow rate 40L / min, powder feeding rate 40g / min, and spraying distance 100mm.

[0080] The yttrium oxide layer is 8 μm thick.

[0081] Performance testing: Coating bond strength: The interfacial bond strength between the coating and the substrate was determined by tensile testing according to ASTM C633.

[0082] Anti-plasma corrosion performance: The sample was placed in an ICP etching machine, using a CF4 / Ar / O2 mixed gas, a power of 1.5kW, a gas pressure of 10Pa, and an etching time of 2h. The corrosion weight loss and surface morphology changes were measured.

[0083] Thermal cycling flatness change: The sample was placed on a 200℃ heating plate and kept at that temperature for 30 minutes, then air-cooled to room temperature. The cycle was repeated 50 times, and the flatness change before and after the cycle was measured using a laser flatness meter.

[0084] The test results are shown in Table 1 below.

[0085] Table 1 Performance Test Data of Aluminum Alloy Forgings for Gas Distribution Discs

[0086] Bond strength / MPa <![CDATA[Plasma etching weight loss / mg / cm 2 > Flatness change after thermal cycling / μm Example 1 38.2 0.12 6.2 Example 2 37.5 0.14 7.0 Comparative Example 1 22.5 0.85 24.5 Comparative Example 2 29.6 0.34 9.8 Comparative Example 3 35.8 0.56 8.5 Comparative Example 4 18.4 0.28 7.2

[0087] Conclusion: The comparative data of the above embodiments and comparative examples show that the aluminum alloy forging of the gas distribution disk prepared by the present invention is significantly superior to the comparative examples in terms of coating bonding strength, plasma corrosion resistance, particle control, and thermal dimensional stability. This fully verifies the advanced nature, synergy, and engineering feasibility of the technical solution of the present invention, and can effectively meet the service requirements of long life, high cleanliness, and dimensional stability of the gas distribution disk of semiconductor equipment in harsh etching environments.

[0088] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, it is intended that all variations falling within the meaning and scope of equivalents of the claims be included within the present invention.

Claims

1. A manufacturing process for an aluminum alloy forging of a gas distribution disk for semiconductor devices, characterized in that: Includes the following steps: S1: Graded homogenization treatment: Using Al 6061 aluminum alloy bars as raw materials, first heat them at 450-455℃ for 5-5.5h, then heat them to 550-555℃ for 24h to obtain homogenized bars. S2: Three-stage free forging: First, an upsetting process is performed; then, a V-shaped anvil forging process is used for drawing; the die is preheated to 250-255℃ and a die finishing process is performed to obtain the forging billet; S3: T652 heat treatment: The forged billet is subjected to solution treatment, water quenching, cold pressing, artificial aging, and air cooling to room temperature in sequence to obtain the uniform gas disk aluminum alloy forging base; S4: Plasma spraying: Plasma spraying is used to deposit a high-entropy alloy support bottom layer and a yttrium oxide surface layer on the surface of the gas distribution plate aluminum alloy forging substrate, and air-cooled to room temperature to obtain the gas distribution plate aluminum alloy forging for semiconductor equipment. During the plasma spraying process, the substrate temperature is stabilized at 150-180℃ by air cooling; The high-entropy alloy support substrate material is pretreated AlCoCrFeNi high-entropy alloy powder obtained by two plasma spraying-quenching cycles, with a particle size of 15-20 μm; the yttrium oxide surface material is yttrium oxide powder with a particle size of 15-45 μm.

2. The manufacturing process of an aluminum alloy forging for a gas distribution disk for semiconductor equipment according to claim 1, characterized in that: The method for preparing the pretreated AlCoCrFeNi high-entropy alloy powder. The process includes the following steps: Step 1: Dry the AlCoCrFeNi high-entropy alloy powder in an argon atmosphere at 150-155℃ for 30-45 minutes to obtain powder A; Step 2: Spray powder A into distilled water coolant, collect the deposited powder, filter, ultrasonically clean, dry, and sieve. Repeat the above steps once to obtain pretreated AlCoCrFeNi high-entropy alloy powder.

3. The manufacturing process of an aluminum alloy forging for a gas distribution disk for semiconductor equipment according to claim 2, characterized in that: During the preparation of pretreated AlCoCrFeNi high-entropy alloy powder, the spraying parameters are as follows: power 32-34kW, voltage 60V, current 520A, spray gun distance 180-200mm, powder feeding rate 4-4.2L / min, argon flow rate 0-40L / min, and hydrogen flow rate 30-32L / min.

4. The manufacturing process of an aluminum alloy forging for a gas distribution disk for semiconductor equipment according to claim 1, characterized in that: In the preparation process of aluminum alloy forgings for gas distribution discs for semiconductor equipment, the plasma spraying parameters for the high-entropy alloy support underlayer are: power 80-90kW, argon flow rate 180-220L / min, hydrogen flow rate 40-60L / min, powder feeding rate 45-60g / min, and spraying distance 100-120mm.

5. The manufacturing process of an aluminum alloy forging for a gas distribution disk for semiconductor equipment according to claim 1, characterized in that: In the preparation process of aluminum alloy forgings for gas distribution discs for semiconductor equipment, the plasma spraying parameters for yttrium oxide surface layer are as follows: power 65-75kW, argon flow rate 160-200L / min, hydrogen flow rate 30-50L / min, powder feeding rate 35-50g / min, and spraying distance 90-110mm.

6. The manufacturing process of an aluminum alloy forging for a gas distribution disk for semiconductor equipment according to claim 1, characterized in that: The supporting substrate has a thickness of 20-30 μm, the yttrium oxide surface layer has a thickness of 5-10 μm, and the total coating thickness is 25-40 μm.

7. The manufacturing process of an aluminum alloy forging for a gas distribution disk for semiconductor equipment according to claim 1, characterized in that: During the upsetting process, the forging temperature is 415-425℃, the total reduction is 35%, the forging speed is 28-32mm / s, and the single-pass reduction is ≤15%. During the drawing process, the forging temperature is 375-385℃, the single-pass pressing and turning angle is 90°, the feed ratio is 0.7, and the forging temperature difference is controlled to be ≤15℃. During the finishing process of the mold, the temperature is 345-355℃, the pressure is 48-50MPa, and the holding time is 14-16s.

8. The manufacturing process of an aluminum alloy forging for a gas distribution disk for semiconductor equipment according to claim 1, characterized in that: The solution treatment parameters are: temperature 475-480℃, time 2.5-3h; the quenching parameters are: temperature 62-68℃, transfer time ≤8s; the cold pressing parameters are: applying 1.8-2.2% permanent deformation perpendicular to the main direction of the free forging streamline at room temperature, at a rate of 0.5-0.55mm / s; the artificial aging parameters are: temperature 120-125℃, time 24h.

9. The aluminum alloy forging for a gas distribution disk for semiconductor equipment prepared by the manufacturing process described in claims 1-8.