A titanium gas distribution plate and its processing technology

Abstract

The present invention provides a titanium gas distribution plate and a processing technology thereof. The process comprises the following steps: (1) heat treating titanium metal, and then mechanically processing to obtain a gas distribution plate blank; (2) electrolytically polishing and cleaning the gas distribution plate blank obtained in step (1) to obtain the gas distribution plate. The present invention designs a gas distribution plate product formed by titanium alloy processing by adjusting the main material of the product, which makes up for the problems of low life and difficulty in recycling of aluminum products, while reducing ion precipitation in the process and improving the chip process yield.

Description

Technical Field

[0001] The invention belongs to the technical field of semiconductor component manufacturing, and relates to a gas distribution plate, and in particular to a titanium gas distribution plate and a processing technology thereof. Background Art

[0002] The gas distribution plate is a commonly used semiconductor component used in the reaction chamber of semiconductor equipment. After passing through the gas distribution plate, the etching gas can evenly reach the wafer surface, react with the wafer surface, and etch out the required circuit pattern.

[0003] Chemical vapor deposition (CVD) is one of the core processes in the production of integrated circuits. Due to its significant advantages in film uniformity, density, coverage, etc., it is widely used in the production of advanced large-scale integrated circuits. The basic principle of CVD is to mix a variety of semiconductor gaseous raw materials evenly, and then introduce them into the reaction chamber at a uniform speed through a gas distribution plate. Under the action of temperature or electric field and pressure, chemical reactions occur between them to form a new thin film material that is deposited on the surface of the wafer. However, the film generated during the reaction will not only be deposited on the bottom wafer, but also on other components of the reaction chamber. The surface of the gas distribution plate, which is the final gas distribution, is more obvious. Therefore, it is particularly important to regularly clean the gas distribution plate components, and a certain degree of cleanliness needs to be maintained. Otherwise, when the surface material is deposited to a certain extent, it will directly fall onto the wafer surface. To ensure product safety, production needs to be stopped frequently to disassemble and clean components. However, since some strong acid and alkali substances are used to clean such attachments, these chemical cleaning agents can easily react with the aluminum matrix material commonly used in gas distribution plates, causing the core microporous area to be easily corroded by the reaction, resulting in dimensional deviations and unevenness, and ultimately causing the product to be scrapped.

[0004] At present, precision semiconductor parts of the gas distribution plate type are mainly made of aluminum alloy. By selecting suitable aluminum alloy materials, processing, forming, surface treatment, cleaning and other processes, and coordinating certain testing operations, they are finally processed into a qualified semiconductor gas distribution plate product; but as the product is used, pollutants will adhere to the surface of equipment parts, especially the parts in the chamber, which are directly exposed to the process reaction, and the surface will adsorb a variety of by-products. In order to ensure the manufacturing yield and process stability, it is necessary to clean the parts in stages to effectively control pollutants. Aluminum products are more reactive and easily react with some cleaning agents, resulting in product size deviations and affecting reuse.

[0005] CN 201066682Y discloses a gas distribution plate for semiconductor equipment, which includes two gas injection tubes, each of which is installed at the center of the gas distribution plate. However, the corrosion resistance of the gas distribution plate is not involved.

[0006] CN 101898890A discloses an alumina ceramic for semiconductor equipment and a preparation process. Without increasing the existing production cost, a trace amount (300-3000ppm) of barium oxide is added to make the sintered high-purity alumina ceramic stable and uniform in the frequency band of 2MHz to 4.8GHz, which does not change with the batch of materials or the position of the blank after sintering, and is less than 3.0×10 -4 The dielectric loss coefficient of this ceramic sintered body can be used to make various key components of semiconductor vacuum manufacturing equipment, such as gas nozzles, gas distribution plates, reaction chamber walls and fixed rings for fixing wafers of plasma equipment. However, the cost of this ceramic material is high and it is not suitable for large-scale promotion.

[0007] CN 114686787A discloses a 6061 aluminum alloy containing a granular iron-rich phase, a preparation method thereof, and a gas distribution plate. The gas distribution plate is prepared by improving the corrosion resistance of the aluminum alloy. The preparation method of the 6061 aluminum alloy containing a granular iron-rich phase comprises the following steps: (1) homogenizing annealing a 6061 aluminum alloy billet to obtain a billet after homogenization annealing; (2) the billet after homogenization annealing is subjected to a first preheating and a first heat preservation and then subjected to at least three The forged billet is subjected to a second forging to obtain a forged billet; (3) the forged billet is subjected to heat treatment annealing to obtain a heat treatment annealed billet; (4) the heat treatment annealed billet is subjected to a second preheating and a second heat preservation, and then hot rolling to obtain a hot rolled billet; (5) the hot rolled billet is subjected to a solid solution treatment and cooling in sequence, and then cold rolling to obtain a cold rolled billet; (6) the cold rolled billet is subjected to aging treatment and leveling in sequence to obtain a 6061 aluminum alloy containing a granular iron-rich phase. Although the aluminum alloy provided by the patent has improved brain corrosion resistance, the preparation process of the aluminum alloy is complicated and is not suitable for large-scale promotion.

[0008] In summary, providing a conventional metal material combined with a specific preparation process to prepare a corrosion-resistant gas distribution plate so that it can be promoted on a large scale has become one of the problems that need to be solved urgently in this field. Summary of the invention

[0009] In view of the shortcomings of the prior art, the purpose of the present invention is to provide a titanium gas distribution plate and a processing technology thereof. The processing technology uses high-purity titanium as a preparation raw material, which makes up for the problems of low life and difficulty in recycling of aluminum products, while reducing ion precipitation in the process and improving the chip process yield.

[0010] To achieve this object, the present invention adopts the following technical solutions:

[0011] In a first aspect, the present invention provides a processing technology for a titanium gas distribution plate, the processing technology comprising the following steps:

[0012] (1) heat treating titanium metal and then machining it to obtain a gas distribution disk blank;

[0013] (2) The gas distribution disk blank obtained in step (1) is subjected to electrolytic polishing and cleaning treatment in sequence to obtain the gas distribution disk.

[0014] The processing technology provided by the present invention adjusts the main material of the product to design a gas distribution plate product formed by titanium alloy, which makes up for the problems of low life and difficulty in recycling of aluminum products, while reducing ion precipitation in the process and improving the chip process yield.

[0015] The processing technology provided by the present invention uses high-purity titanium material for the manufacture of semiconductor gas distribution plates through the adjustment and precise control of the material, which can not only avoid the precipitation of aluminum ions in aluminum alloys and the influence of impurity elements in aluminum alloys on chip manufacturing, but also the excellent corrosion resistance of titanium material can effectively avoid the change of product precision hole size due to chemical corrosion when the subsequent gas distribution plate is repeatedly cleaned and used, thereby effectively extending the service life of the product and ensuring the process stability of the chip manufacturing process, without the need to repeatedly adjust the corresponding flow rate and other parameters according to the change of product size.

[0016] Preferably, the purity of the metallic titanium in step (1) is ≥99.9%, for example, it can be 99.9%, 99.92%, 99.94%, 99.96% or 99.98%, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0017] Preferably, the temperature of the heat treatment in step (1) is 500-550°C, for example, it can be 500°C, 510°C, 520°C, 530°C, 540°C or 550°C, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0018] Preferably, the heat treatment time in step (1) is 2 to 4 h, for example, it can be 2 h, 2.2 h, 2.4 h, 2.6 h, 2.8 h, 3 h, 3.2 h, 3.4 h, 3.6 h, 3.8 h or 4 h, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0019] The purity of the titanium metal described in the present invention is ≥99.9%, and the total impurity content is <0.1%, and the reasons are as follows: the higher the purity of the titanium metal, the fewer impurity element particles in the product; however, the impurity element particles have a very significant effect on the physical, chemical properties, mechanical properties and corrosion resistance of the material, especially some interstitial impurities, which will cause the titanium grains to distort, thereby affecting the physical, chemical, mechanical and corrosion resistance of titanium. Under normal temperature conditions, the possibility of titanium and other substances reacting is small, but when the temperature is raised to a certain level, these impurity positions may easily become the breakthrough point of the reaction, and long-term accumulation will cause abnormal use of the product; in addition, the mechanical processing of titanium materials also needs to control a certain purity and cost. The higher the purity, the lower the hardness of the corresponding material, and the more convenient the processing, but the material cost will become much larger. After comprehensive consideration, 99.9% high-purity titanium can be selected as a more appropriate choice.

[0020] Preferably, the mechanical processing in step (1) is: cutting, grinding and polishing the metal titanium in sequence according to the target size to obtain a gas distribution plate blank.

[0021] Preferably, the rotation speed during the cutting process is 2000-8000 r / min, for example, it can be 2000 r / min, 3000 r / min, 4000 r / min, 5000 r / min, 6000 r / min, 7000 r / min or 8000 r / min, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0022] Preferably, the feed rate in the cutting process is 400-1000 m / min, for example, it can be 400 m / min, 500 m / min, 600 m / min, 700 m / min, 800 m / min, 900 m / min or 1000 m / min, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0023] Preferably, the feed amount in the cutting process is 0.1-0.5 mm, for example, 0.1 mm, 0.2 mm, 0.3 mm, 0.4 mm or 0.5 mm, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0024] Preferably, the tool used in the cutting process includes a tungsten steel milling cutter.

[0025] The present invention adopts a tungsten steel milling cutter to cut metal titanium, and can improve the machining quality and efficiency by controlling the rotation speed, feed rate and feed rate during the cutting process.

[0026] Preferably, the rotation speed during the grinding process is 2000-5000 r / min, for example, it can be 2000 r / min, 3000 r / min, 4000 r / min or 5000 r / min, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0027] Preferably, the cutting speed in the grinding process is 30 to 100 m / min, for example, 30 m / min, 40 m / min, 50 m / min, 60 m / min, 70 m / min, 80 m / min, 90 m / min or 100 m / min, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0028] Preferably, the cutting depth during the grinding process is 0.1-0.5 m / min, for example, it can be 0.1 m / min, 0.2 m / min, 0.3 m / min, 0.4 m / min or 0.5 m / min, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0029] Preferably, the feed rate during the grinding process is 0.1-0.5 mm / r, for example, it can be 0.1 mm / r, 0.2 mm / r, 0.3 mm / r, 0.4 mm / r or 0.5 mm / r, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0030] Preferably, the tool used in the grinding process comprises a cemented carbide tool.

[0031] Preferably, the cemented carbide tool is provided with a TiC coating.

[0032] Preferably, the polishing includes sequentially using 400# water-based sandpaper, 1000# water-based sandpaper and 2000# water-based sandpaper to polish until the surface is bright.

[0033] Preferably, the grinding time is 2 to 4 minutes, for example, 2 minutes, 2.5 minutes, 3 minutes or 4 minutes, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0034] Preferably, the polishing wetting agent comprises water and / or ethanol.

[0035] Preferably, after the grinding, the process further comprises rinsing the surface of the gas distribution plate blank with water and drying it.

[0036] Preferably, the electrolytic polishing solution used in the electrolytic polishing in step (2) comprises, by volume percentage: 5-15% perchloric acid, 55-65% ethanol, 5-15% n-butanol and 15-30% water.

[0037] Preferably, the electrolytic polishing time in step (2) is 35 to 45 s, for example, 35 s, 36 s, 37 s, 38 s, 39 s, 40 s, 41 s, 42 s, 43 s, 44 s or 45 s, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0038] Preferably, the voltage of the electrolytic polishing in step (2) is 30 to 40 V, for example, 30 V, 32 V, 34 V, 36 V, 38 V or 40 V, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0039] Preferably, the cleaning process in step (2) includes a primary cleaning and a secondary cleaning performed sequentially.

[0040] Preferably, the one-time cleaning includes degreasing cleaning, chemical cleaning and passivation performed in sequence.

[0041] The purpose of the degreasing cleaning described in the present invention is to remove grease from the metal surface, provide a clean metal surface for subsequent operation procedures, and also prevent excessive dirt on the product surface from affecting the quality and service life of the subsequent cleaning liquid; the purpose of the chemical cleaning is to remove a layer of oxide layer on the product surface to expose the relatively pure metal at the bottom; the purpose of the passivation is to convert the metal surface of the product into a state that is not easily oxidized, thereby improving the corrosion resistance of the titanium metal surface and improving the performance of the product.

[0042] Preferably, the chemical cleaning is to place the blank in a chemical reagent for immersion cleaning.

[0043] Preferably, the chemical reagent comprises hydrofluoric acid and nitric acid.

[0044] Preferably, the mass concentration of the hydrofluoric acid is 1-3%, for example, 1%, 1.4%, 1.8%, 2.2%, 2.6% or 3%, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0045] Preferably, the mass concentration of the nitric acid is 15-25%, for example, 15%, 17%, 19%, 21%, 23% or 25%, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0046] Preferably, the immersion cleaning temperature is 10-30°C, for example, 10°C, 14°C, 18°C, 22°C, 26°C or 30°C, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0047] Preferably, the immersion cleaning time is 2 to 5 minutes, for example, it can be 2 minutes, 2.3 minutes, 2.6 minutes, 2.9 minutes, 3.2 minutes, 3.5 minutes, 3.8 minutes, 4.1 minutes, 4.4 minutes, 4.7 minutes or 5 minutes, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0048] Preferably, the passivation agent used in the passivation comprises a nitric acid solution.

[0049] Preferably, the concentration of the nitric acid solution is 30-50wt%, for example, 30wt%, 34wt%, 38wt%, 42wt%, 46wt% or 50wt%, but is not limited to the values ​​listed.

[0050] Preferably, the passivation time is 3 to 10 minutes, for example, 3 minutes, 4 minutes, 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes or 10 minutes, but is not limited to the listed values, and other values ​​not listed within the numerical range are also applicable.

[0051] Preferably, the secondary cleaning includes a first high-pressure water cleaning, an ultrasonic cleaning and a second high-pressure water cleaning performed in sequence.

[0052] The invention can remove chemical residues, dust and dirty residues in difficult-to-clean structural positions such as some gaps and corners on the product surface through high-pressure water washing.

[0053] In addition, the high-pressure water washing of the present invention is more efficient than immersion cleaning, and the requirements for water quality are also reduced, thereby making the production process easier to operate.

[0054] Preferably, the ultrasonic cleaning is performed 1 to 4 times, for example, 1 time, 2 times, 3 times or 4 times.

[0055] Preferably, the water pressure in the first high-pressure water flushing and the second high-pressure water flushing is 0.3-0.6 MPa, for example, it can be 0.3 MPa, 0.4 MPa, 0.5 MPa or 0.6 MPa, but is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0056] As a preferred technical solution of the present invention, the processing technology of the titanium gas distribution plate provided in the first aspect of the present invention comprises the following steps:

[0057] (1) heat treating metallic titanium with a purity of ≥99.9% at 500-550° C. for 2-4 hours, and then mechanically processing to obtain a gas distribution disk blank;

[0058] The mechanical processing is as follows: cutting, grinding and polishing the metal titanium in sequence according to the target size to obtain a gas distribution plate blank;

[0059] The tool used in the cutting process is a tungsten steel milling cutter, the rotation speed is 2000-8000r / min, the feed rate is 400-1000m / min, and the feed amount is 0.1-0.5mm;

[0060] The tool used in the grinding process is a cemented carbide tool provided with a TiC coating, with a rotation speed of 2000-5000 r / min, a cutting speed of 30-100 m / min, a cutting depth of 0.1-0.5 m / min, and a feed rate of 0.1-0.5 mm / r;

[0061] The polishing includes sequentially using 400# water-based sandpaper, 1000# water-based sandpaper and 2000# water-based sandpaper to polish for 2 to 4 minutes until the surface is bright;

[0062] (2) subjecting the gas distribution disk blank obtained in step (1) to electrolytic polishing and cleaning in sequence to obtain the gas distribution disk;

[0063] The electrolytic polishing time is 35 to 45 seconds, the voltage is 30 to 40 V, and the electrolytic polishing solution used includes, by volume percentage: 5 to 15% perchloric acid, 55 to 65% ethanol, 5 to 15% n-butanol and 15 to 30% water;

[0064] The cleaning process includes a primary cleaning and a secondary cleaning performed sequentially;

[0065] The one-time cleaning includes degreasing cleaning performed in sequence, using chemical reagents for immersion cleaning at a temperature of 10 to 30° C. for 2 to 5 minutes, and then passivating treatment with a nitric acid solution with a concentration of 30 to 50 wt% for 3 to 10 minutes; the chemical reagents contain hydrofluoric acid with a mass concentration of 1 to 3% and nitric acid with a mass concentration of 15 to 25%;

[0066] The secondary cleaning includes a first high-pressure water rinse, ultrasonic cleaning 1 to 4 times and a second high-pressure water rinse performed in sequence; the water pressure in the first high-pressure water rinse and the second high-pressure water rinse is 0.3 to 0.6 MPa.

[0067] In a second aspect, the present invention provides a titanium gas distribution plate, wherein the titanium gas distribution plate is obtained by using the processing technology provided in the first aspect.

[0068] The numerical range described in the present invention not only includes the point values ​​listed above, but also includes any point values ​​between the above numerical ranges that are not listed. Due to space limitations and for the sake of simplicity, the present invention no longer exhaustively lists the specific point values ​​included in the range.

[0069] Compared with the prior art, the present invention has the following beneficial effects:

[0070] The processing technology provided by the present invention uses high-purity titanium material for the manufacture of semiconductor gas distribution plates through the adjustment and precise control of the material, which can not only avoid the precipitation of aluminum ions in aluminum alloys and the influence of impurity elements in aluminum alloys on chip manufacturing, but also the excellent corrosion resistance of titanium material can effectively avoid the change of product precision hole size due to chemical corrosion when the subsequent gas distribution plate is repeatedly cleaned and used, thereby effectively extending the service life of the product and ensuring the process stability of the chip manufacturing process, without the need to repeatedly adjust the corresponding flow rate and other parameters according to the change of product size. DETAILED DESCRIPTION

[0071] The technical solution of the present invention is further described below by specific implementation methods. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0072] Example 1

[0073] This embodiment provides a titanium gas distribution plate, and the processing technology of the titanium gas distribution plate includes the following steps:

[0074] (1) heat treating metallic titanium with a purity of ≥99.9% at 525° C. for 3 h, and then machining to obtain a gas distribution disk blank;

[0075] The mechanical processing is as follows: cutting, grinding and polishing the metal titanium in sequence according to the target size to obtain a gas distribution plate blank;

[0076] The tool used in the cutting process is a tungsten steel milling cutter, with a rotation speed of 6000r / min, a feed rate of 800m / min, and a feed rate of 0.3mm;

[0077] The tool used in the grinding process is a cemented carbide tool provided with a TiC coating, with a rotation speed of 3500 r / min, a cutting speed of 80 m / min, a cutting depth of 0.35 m / min, and a feed rate of 0.35 mm / r;

[0078] The polishing includes sequentially using 400# water-based sandpaper, 1000# water-based sandpaper and 2000# water-based sandpaper to polish for 3 minutes until the surface is bright;

[0079] (2) subjecting the gas distribution disk blank obtained in step (1) to electrolytic polishing and cleaning in sequence to obtain the gas distribution disk;

[0080] The electrolytic polishing time is 40s, the voltage is 35V, and the electrolytic polishing solution used includes, by volume percentage: 10% perchloric acid, 60% ethanol, 10% n-butanol and 20% water;

[0081] The cleaning process includes a primary cleaning and a secondary cleaning performed sequentially;

[0082] The one-time cleaning includes degreasing cleaning performed in sequence, using a chemical reagent for immersion cleaning at a temperature of 25° C. for 4 minutes, and then passivating treatment for 6 minutes using a nitric acid solution with a concentration of 40wt%; the chemical reagent contains hydrofluoric acid with a mass concentration of 2% and nitric acid with a mass concentration of 20%;

[0083] The secondary cleaning includes a first high-pressure water rinse, three ultrasonic rinses, and a second high-pressure water rinse performed in sequence; the water pressure in the first high-pressure water rinse and the second high-pressure water rinse is 0.45 MPa.

[0084] Example 2

[0085] This embodiment provides a titanium gas distribution plate, and the processing technology of the titanium gas distribution plate includes the following steps:

[0086] (1) heat treating metallic titanium with a purity of ≥99.9% at 550° C. for 2 h, and then machining to obtain a gas distribution disk blank;

[0087] The mechanical processing is as follows: cutting, grinding and polishing the metal titanium in sequence according to the target size to obtain a gas distribution plate blank;

[0088] The tool used in the cutting process is a tungsten steel milling cutter, with a rotation speed of 2000r / min, a feed rate of 400m / min, and a feed rate of 0.1mm;

[0089] The tool used in the grinding process is a cemented carbide tool provided with a TiC coating, with a rotation speed of 2000 r / min, a cutting speed of 30 m / min, a cutting depth of 0.1-m / min, and a feed rate of 0.1 mm / r;

[0090] The polishing includes sequentially using 400# water-based sandpaper, 1000# water-based sandpaper and 2000# water-based sandpaper to polish for 4 minutes until the surface is bright;

[0091] (2) subjecting the gas distribution disk blank obtained in step (1) to electrolytic polishing and cleaning in sequence to obtain the gas distribution disk;

[0092] The electrolytic polishing time is 35s, the voltage is 40V, and the electrolytic polishing solution used includes, by volume percentage: 5% perchloric acid, 65% ethanol, 5% n-butanol and 25% water;

[0093] The cleaning process includes a primary cleaning and a secondary cleaning performed sequentially;

[0094] The one-time cleaning includes degreasing cleaning performed in sequence, using a chemical reagent for immersion cleaning at a temperature of 10° C. for 5 minutes, and then passivating treatment with a 30wt% nitric acid solution for 10 minutes; the chemical reagent contains hydrofluoric acid with a mass concentration of 3% and nitric acid with a mass concentration of 15%;

[0095] The secondary cleaning includes a first high-pressure water rinse, four ultrasonic rinses, and a second high-pressure water rinse performed in sequence; the water pressure in the first high-pressure water rinse and the second high-pressure water rinse is 0.6 MPa.

[0096] Example 3

[0097] This embodiment provides a titanium gas distribution plate, and the processing technology of the titanium gas distribution plate includes the following steps:

[0098] (1) heat treating metallic titanium with a purity of ≥99.9% at 500° C. for 4 h, and then machining to obtain a gas distribution disk blank;

[0099] The mechanical processing is as follows: cutting, grinding and polishing the metal titanium in sequence according to the target size to obtain a gas distribution plate blank;

[0100] The tool used in the cutting process is a tungsten steel milling cutter, with a rotation speed of 8000r / min, a feed rate of 1000m / min, and a feed rate of 0.5mm;

[0101] The tool used in the grinding process is a cemented carbide tool provided with a TiC coating, with a rotation speed of 5000 r / min, a cutting speed of 100 m / min, a cutting depth of 0.5 m / min, and a feed rate of 0.5 mm / r;

[0102] The polishing includes sequentially using 400# water-based sandpaper, 1000# water-based sandpaper and 2000# water-based sandpaper to polish for 2 minutes until the surface is bright;

[0103] (2) subjecting the gas distribution disk blank obtained in step (1) to electrolytic polishing and cleaning in sequence to obtain the gas distribution disk;

[0104] The electrolytic polishing time is 45 seconds, the voltage is 30V, and the electrolytic polishing solution used includes, by volume percentage: 15% perchloric acid, 55% ethanol, 15% n-butanol and 15% water;

[0105] The cleaning process includes a primary cleaning and a secondary cleaning performed sequentially;

[0106] The one-time cleaning includes degreasing cleaning performed in sequence, using a chemical reagent to soak and clean for 2 minutes at a temperature of 30° C., and then passivating for 3 minutes using a 50wt% nitric acid solution; the chemical reagent contains hydrofluoric acid with a mass concentration of 1% and nitric acid with a mass concentration of 25%;

[0107] The secondary cleaning includes a first high-pressure water rinse, an ultrasonic rinse once, and a second high-pressure water rinse performed in sequence; the water pressure in the first high-pressure water rinse and the second high-pressure water rinse is 0.3 MPa.

[0108] Example 4

[0109] This embodiment provides a titanium gas distribution plate. The processing technology of the titanium gas distribution plate is different from that of the embodiment 1 only in that:

[0110] In this embodiment, the temperature of the heat treatment in step (1) is changed to 450°C.

[0111] Example 5

[0112] This embodiment provides a titanium gas distribution plate. The processing technology of the titanium gas distribution plate is different from that of the embodiment 1 only in that:

[0113] In this embodiment, the temperature of the heat treatment in step (1) is changed to 580°C.

[0114] Example 6

[0115] This embodiment provides a titanium gas distribution plate. The processing technology of the titanium gas distribution plate is different from that of the embodiment 1 only in that:

[0116] In this embodiment, the purity of the metallic titanium in step (1) is changed to 85%.

[0117] Example 7

[0118] This embodiment provides a titanium gas distribution plate. The processing technology of the titanium gas distribution plate is different from that of the embodiment 1 only in that:

[0119] In this embodiment, the grinding process in the mechanical processing described in step (1) is omitted.

[0120] Example 8

[0121] This embodiment provides a titanium gas distribution plate. The processing technology of the titanium gas distribution plate is different from that of the embodiment 1 only in that:

[0122] In this embodiment, the polishing in step (1) is changed to using only 2000# water-based sandpaper for polishing.

[0123] Example 9

[0124] This embodiment provides a titanium gas distribution plate. The processing technology of the titanium gas distribution plate is different from that of the embodiment 1 only in that:

[0125] In this embodiment, the voltage of the electrolytic polishing in step (2) is changed to 25V.

[0126] Example 10

[0127] This embodiment provides a titanium gas distribution plate. The processing technology of the titanium gas distribution plate is different from that of the embodiment 1 only in that:

[0128] In this embodiment, the voltage of the electrolytic polishing in step (2) is changed to 50V.

[0129] Embodiment 11

[0130] This embodiment provides a titanium gas distribution plate. The processing technology of the titanium gas distribution plate is different from that of the embodiment 1 only in that:

[0131] In this embodiment, the cleaning step (2) is omitted.

[0132] Example 12

[0133] This embodiment provides a titanium gas distribution plate. The processing technology of the titanium gas distribution plate is different from that of the embodiment 1 only in that:

[0134] In this embodiment, the high-pressure water flushing described in step (2) is omitted.

[0135] Comparative Example 1

[0136] This comparative example provides a gas distribution plate, and the processing technology of the gas distribution plate is different from that of Example 1 only in that:

[0137] In this comparative example, the metal titanium in step (1) is replaced by metal aluminum.

[0138] Comparative Example 2

[0139] This comparative example provides a titanium gas distribution plate, and the processing technology of the titanium gas distribution plate is different from that of Example 1 only in that:

[0140] In this comparative example, the heat treatment described in step (1) was omitted.

[0141] Performance testing:

[0142] The titanium gas distribution plates provided in Examples 1-12 and Comparative Examples 1-2 were subjected to performance tests, including roughness tests and particle size tests, and the results are shown in Table 1.

[0143] Table 1

[0144]

[0145] In summary, the present invention designs a gas distribution plate product formed by titanium alloy by adjusting the main material of the product, which makes up for the problems of low life and difficulty in recycling of aluminum products, while reducing ion precipitation in the process and improving the chip process yield.

[0146] The specific embodiments described above further illustrate the objectives, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above description is only a specific embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A processing technology for a titanium gas distribution plate, characterized in that: The process comprises the following steps: (1) heat treating metallic titanium with a purity of ≥99.9% at 500-550° C., and then mechanically processing the metal to obtain a gas distribution disk blank; The mechanical processing is as follows: cutting, grinding and polishing the metal titanium in sequence according to the target size to obtain a gas distribution plate blank; (2) subjecting the gas distribution disk blank obtained in step (1) to electrolytic polishing and cleaning in sequence to obtain the gas distribution disk; Wherein, the cleaning process includes a primary cleaning and a secondary cleaning performed sequentially; The one-time cleaning includes degreasing cleaning, chemical cleaning and passivation performed in sequence; The secondary cleaning includes a first high-pressure water cleaning, an ultrasonic cleaning and a second high-pressure water cleaning performed in sequence.

2. The processing technology according to claim 1, characterized in that: The heat treatment time in step (1) is 2 to 4 hours.

3. The processing technology according to claim 1, characterized in that: The rotation speed during the cutting process is 2000-8000 r / min.

4. The processing technology according to claim 1, characterized in that: The feed rate during the cutting process is 400-1000 m / min.

5. The processing technology according to claim 1, characterized in that: The feed amount during the cutting process is 0.1-0.5 mm.

6. The processing technology according to claim 1, characterized in that: The cutting tool used in the cutting process includes a tungsten steel milling cutter.

7. The processing technology according to claim 1, characterized in that: The rotation speed during the grinding process is 2000-5000 r / min.

8. The processing technology according to claim 1, characterized in that: The cutting speed during the grinding process is 30-100 m / min.

9. The processing technology according to claim 1, characterized in that: The cutting depth during the grinding process is 0.1-0.5 m / min.

10. The processing technology according to claim 1, characterized in that: The feed rate during the grinding process is 0.1-0.5 mm / r.

11. The processing technology according to claim 1, characterized in that: The cutting tools used in the grinding process include cemented carbide cutting tools.

12. The processing technology according to claim 11, characterized in that: The cemented carbide tool is provided with a TiC coating.

13. The processing technology according to claim 1, characterized in that: The polishing includes sequentially using 400# water-based sandpaper, 1000# water-based sandpaper and 2000# water-based sandpaper to polish until the surface is bright.

14. The processing technology according to claim 13, characterized in that: The grinding time is 2 to 4 minutes.

15. The processing technology according to claim 1, characterized in that: The polishing wetting agent includes water and / or ethanol.

16. The processing technology according to claim 1, characterized in that: After the grinding, the process also includes washing the surface of the gas distribution plate blank with water and drying it.

17. The processing technology according to claim 1, characterized in that: The electrolytic polishing solution used in the electrolytic polishing of step (2) comprises, by volume percentage: 5-15% perchloric acid, 55-65% ethanol, 5-15% n-butanol and 15-30% water.

18. The processing technology according to claim 1, characterized in that: The electrolytic polishing time in step (2) is 35 to 45 seconds.

19. The processing technology according to claim 1, characterized in that: The voltage of the electrolytic polishing in step (2) is 30 to 40V.

20. The processing technology according to claim 1, characterized in that: The chemical cleaning is to place the blank in a chemical reagent and soak it for cleaning.

21. The processing technology according to claim 20, characterized in that: The chemical reagents include hydrofluoric acid and nitric acid.

22. The processing technology according to claim 21, characterized in that: The mass concentration of the hydrofluoric acid is 1-3%.

23. The processing technology according to claim 21, characterized in that: The mass concentration of the nitric acid is 15-25%.

24. The processing technology according to claim 20, characterized in that: The temperature of the immersion cleaning is 10-30°C.

25. The processing technology according to claim 20, characterized in that: The soaking and cleaning time is 2 to 5 minutes.

26. The processing technology according to claim 1, characterized in that: The passivation agent used in the passivation includes a nitric acid solution.

27. The processing technology according to claim 26, characterized in that: The concentration of the nitric acid solution is 30-50 wt %.

28. The processing technology according to claim 1, characterized in that: The passivation time is 3 to 10 minutes.

29. The processing technology according to claim 1, characterized in that: The ultrasonic cleaning is performed 1 to 4 times.

30. The processing technology according to claim 1, characterized in that: The water pressure in the first high-pressure water flushing and the second high-pressure water flushing is 0.3-0.6 MPa.

31. A titanium gas distribution plate, characterized in that: The titanium gas distribution plate is obtained by using the processing technology described in any one of claims 1-30.

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