CN115739819B - Ultra-high clean cleaning process and application of semiconductor device aluminum alloy parts - Google Patents
Ultra-high clean cleaning process and application of semiconductor device aluminum alloy parts Download PDFInfo
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Abstract
The invention discloses an ultra-high clean cleaning process for aluminum alloy parts of semiconductor equipment and application thereof, and relates to the technical field of part cleaning. In this application with aluminum alloy spare part through in the washing liquid, acid etching solution, pickling solution, nitric acid aqueous solution soak the back, continue with high-pressure water washing, hot water washing, overflow hot water soaking, nitrogen gas weathers, toasts etc. handle, can realize fine clean effect with aluminum alloy spare part, make the spare part surface that obtains bright, the color and luster homogeneous, no spot, the mar, and the ion that obtains spare part surface residue, organic matter content are few moreover, can reach the washing standard. In addition, the secondary pollution on the surface of the part after the cleaning is well avoided, and the cleaning agent can be well used for cleaning the aluminum alloy part of the 5-nanometer semiconductor equipment.
Description
Technical Field
The invention relates to the technical field of cleaning of parts, in particular to an ultra-high clean cleaning process and application of an aluminum alloy part of semiconductor equipment.
Background
The aluminum alloy has excellent corrosion resistance, ductility and strength, is one of the light metal materials with the widest application range, and is widely applied to the aspects of aerospace, integrated circuits, national defense and military industry, petrochemical industry, medical appliances and the like. However, an oxide film is formed on the surface of the substrate during the processing process, which prevents the further application of the substrate, and chemical cleaning is a common method for removing the oxide film. The chemical cleaning mainly uses acid as main material, and is synergistic with proper treatment of active agent, penetrant and corrosion inhibitor so as to attain the cleaning effect. In the process of manufacturing semiconductor devices, the cleaning process of aluminum alloy parts is a key for determining the stability, reliability and yield of the devices.
Chinese patent application CN109183114a discloses a hard anodic oxidation process, wherein the workpiece is subjected to degreasing, alkaline biting, acid etching, acid washing, ash removal and four aqueous operations, and then is subjected to oxidation treatment, so that the hard anodic oxidation of the aluminum alloy is realized, and the corrosion resistance time is effectively improved. However, the aluminum alloy surface cleaned by the technical scheme has higher residual metal content. Chinese patent application CN110449407a discloses a process for ultra-clean cleaning of semiconductor aluminum alloy parts, which thoroughly removes dust particles, metal ions, oil stains and dirt by pre-cleaning, acid cleaning, water cleaning and blow-drying the semiconductor aluminum alloy parts. However, the content of the residual metal ions can be further reduced, and the method has weak cleaning effect on organic matters. Accordingly, the applicant has made extensive studies to improve the performance of the present invention, and has made the present application.
Disclosure of Invention
In order to solve the above problems, a first aspect of the present invention provides an ultra-high clean cleaning process for aluminum alloy parts of semiconductor equipment, comprising:
s1, placing a part to be cleaned in an ultrasonic cleaner containing cleaning liquid, heating to 55-65 ℃, cleaning for 2-10 min, and removing oil stains on the surface of the product;
s2, placing the parts obtained after the treatment in the S1 into clean water for first filtering and cleaning to remove residual liquid medicine on the surfaces of the parts;
s3, immersing the parts obtained after the cleaning in the S2 into a container containing an acid etching solution, performing acid etching treatment for 8-18S, removing surface natural oxides, and repeating the step S2;
s4, immersing the parts obtained after the cleaning in the S3 in a container containing an acid washing solution for 1-5 minutes, removing new oxides on the surface, and repeating the step S2;
s5, immersing the parts obtained after the cleaning in the S4 in a nitric acid mixed aqueous solution for 5-10 min, and repeating the step S2;
s6, immersing the parts obtained after the treatment in the S5 in a nitric acid aqueous solution for 1-5min, and repeating the step S2;
s7, washing the parts obtained after the treatment in the S6 with clean water under high pressure, and further removing the liquid medicine attached to the surfaces of the products;
s8, placing the parts obtained after the cleaning in the S7 into an ultrasonic hot water tank with the temperature of 20-30 ℃ for filtering and cleaning for 1-5 min;
s9, overflowing and opening 1/3, and soaking the parts obtained after the S8 cleaning with hot water at 40-46 ℃ for 2-5 min;
s10, drying the parts obtained after the S9 cleaning by adopting nitrogen filtered by a 0.1 mu m filter;
s11, baking the parts obtained after the step S10 is dried in a baking oven filled with nitrogen;
s12, vacuumizing and packaging the parts obtained after the baking in the S11 by using dust-free cloth and packaging bags.
In some preferred embodiments, the cleaning solution in S1 is an aqueous solution containing a cleaning agent and an active agent.
In some preferred embodiments, the concentration of the cleaning agent is 20-50g/L and the mass volume percent concentration of the active agent is 2-30%; preferably, the concentration of the cleaning agent is 30-35g/L, and the mass volume percentage concentration of the active agent is 6-10%.
In some preferred embodiments, the cleaning agent is selected from at least one of sodium hydroxide, potassium hydroxide, sodium phosphate, potassium carbonate, sodium metasilicate, ethylene oxide propylene oxide copolymer, sodium pyrophosphate, potassium tripolyphosphate, borax, polyoxyethylene polyoxypropylene ether; preferably sodium phosphate, borax, sodium carbonate and polyoxyethylene polyoxypropylene ether.
In some preferred embodiments, the concentration percentages of the sodium phosphate, the borax, the sodium carbonate and the polyoxyethylene polyoxypropylene ether in the cleaning agent are (4-5): (2-3): (1.5-2.5): 1, a step of; preferably 4.5:2.5:2:1.
in some preferred embodiments, the active agent is selected from at least one of sodium linear alkylbenzenesulfonate, fatty alcohol polyoxyethylene ether, fatty alcohol thioether sodium, alkylphenol polyoxyethylene ether, alkyl alcohol amide sodium phosphate, fatty amine polyoxyethylene ether; sodium linear alkylbenzene sulfonate and sodium fatty alcohol thioether are preferred.
In some preferred embodiments, the concentration percentage of the linear sodium alkylbenzene sulfonate and the fatty alcohol sodium thioether in the active agent is (2.5-3.5): (1.5-2.5); preferably 3:2.
in some preferred embodiments, the straight-chain hydrocarbon R in the sodium linear alkylbenzenesulfonate is C10-C18; preferably C10 to C16.
In some preferred embodiments, the sodium fatty alcohol thioether has the formula RO (CH) 2 CH 2 O)n-SO 3 Na, wherein n=2-3, and R is C12-15.
According to the invention, the aluminum alloy part is placed in the cleaning liquid, so that impurities such as greasy dirt adhered to the surface of the part can be effectively removed. The applicant finds that the cleaning agent and the active agent are mixed, so that not only can the oil stain impurities on the surface be removed completely, but also the removal efficiency of the cleaning agent can be improved, especially, the active agent is linear sodium alkylbenzenesulfonate and fatty alcohol sodium thioether, and the excellent affinity of hydrophilic groups and lipophilic groups of the active agent is fully utilized in an alkaline environment to arrange the active agent and the fatty alcohol sodium thioether between two phases, so that the surface tension and the surface free energy of an aluminum alloy part are well reduced, the wetting, emulsifying and dispersing effects of the cleaning agent on the surfaces of impurity particles on the surfaces of the part are promoted, and the cleaning and degreasing effects of the cleaning agent are further improved. The applicant has found that, surprisingly, when the concentration of the cleaning agent in the cleaning liquid is 20-50g/L and the mass-volume percentage concentration of the active agent is 2-30%, the surface cleaning effect is improved and the aluminum alloy substrate material is not damaged.
In some preferred embodiments, the resistivity of the water in the S2 is more than or equal to 1MΩ, the spray washing treatment time is 60-120S, and the temperature is 20-30 ℃; preferably, the resistivity of the water in the S2 is more than or equal to 2MΩ, the spray washing treatment time is 90S, and the temperature is 25 ℃.
In some preferred embodiments, the acid etching solution in S3 is an aqueous solution of an acidic substance.
In some preferred embodiments, the acidic substance is selected from at least one of hydrofluoric acid, nitric acid, sulfamic acid, hydrochloric acid, glacial acetic acid, sulfuric acid, oxalic acid; hydrofluoric acid and nitric acid are preferred.
In some preferred embodiments, the mass-volume percentage concentration of hydrofluoric acid in the acid etching solution is 1-10%; preferably 2-5%.
In some preferred embodiments, the mass-volume percentage concentration of the nitric acid in the acid etching solution is 10-30%; preferably 15-25%.
The cleaning liquid can remove impurities such as greasy dirt on the surface of an aluminum alloy part, but has poor effect of removing impurity oxides such as magnesium, silicon, copper, iron and the like adsorbed and fixed on the surface. According to the method, the oxide film on the surface of the part can be further removed by soaking the part in the acid etching solution, particularly, the acid etching solution consisting of 1-10% of hydrofluoric acid and 10-30% of nitric acid is selected, the removal effect is good, si on the surface of the part can be completely removed, metal impurities such as magnesium and copper on the surface can be removed, natural oxides on the surface can be etched away, the surface is continuously prevented from being influenced in the later stage of application of a semiconductor, particularly, the acid etching treatment time is 8-18 s, the surface color is uniform and consistent, no chromatic aberration is generated, and if the acid etching treatment time is too long, the surface of the aluminum alloy part is colored or darkened. However, new oxide films such as magnesium oxide, copper oxide, ferrous oxide and the like are formed on the surfaces of the parts during acid etching treatment, so that the surfaces of the parts are in a fog-white state, fluorescent particles are arranged on the surfaces of the parts after black light detection, and the UHV chemical cleaning requirements cannot be met.
In some preferred embodiments, the acid washing solution in S4 is at least one selected from the group consisting of aqueous hydrochloric acid, aqueous nitric acid, aqueous hydrofluoric acid, aqueous citric acid, aqueous acetic acid, aqueous sulfuric acid, aqueous ozone, and aqueous phosphoric acid; a combination of aqueous nitric acid and aqueous ozone is preferred.
In some preferred embodiments, the mass-volume percentage concentration of the nitric acid in the acid washing solution in the step S4 is 10-30%, and the mass-volume percentage concentration of the ozone is 3-8%; preferably, the mass volume percentage concentration of nitric acid is 15-25%, and the mass volume percentage concentration of ozone is 5%.
The applicant finds that the parts are placed in the acid washing solution, so that newly generated oxide film layers such as magnesium oxide, copper oxide and ferrous oxide generated on the surfaces can be removed, the color of the aluminum alloy is lightened, fluorescent particles existing on the surfaces can be effectively removed, the cleaning effect of the aluminum alloy is improved, and the cleaning effect on organic matters is poor. The applicant has found that, when the pickling solution is a combination of nitric acid aqueous solution and ozone aqueous solution, organic dirt on the surface of the material can be effectively removed, and a hydrophilic compact film can be formed on the surface of the aluminum alloy, so that the surface of the material is prevented from further adsorbing dust particles, metal impurities, organic matters and other polluted foreign matters, and re-pollution of parts is prevented.
In some preferred embodiments, the mass-volume percentage concentration of the nitric acid in the nitric acid mixed aqueous solution in the step S5 is 10-30%; preferably 15-25%.
The method is characterized in that the surface of nearly pure aluminum can be obtained by carrying out extraction treatment on the aluminum alloy part subjected to acid washing by using a nitric acid mixed aqueous solution, particularly, the nitric acid mixed aqueous solution with the mass volume percentage concentration of 10-30% is selected to keep the surface of the part continuous, no spots, color differences and scratches exist, meanwhile, the residual ions on the surface of the material are further removed, the content of various detectable metal cations and anions remained on the surface of the material is within a strict standard range, the content of various detectable organic matters such as cyclotrisiloxane, hexamethyl, alkylphenol, ketone and the like is 1ng/cm 2 Under the condition, the cleaning standard requirements for UHV clean components 0250-20000 is reached.
In some preferred embodiments, the mass-volume percentage concentration of the nitric acid in the nitric acid aqueous solution in S6 is 2-20%; preferably 5-15%.
In some preferred embodiments, the pressure of the high-pressure clean water flushing in the step S7 is 50-300 bar, the straight line distance between the gun head of the water gun and the parts is 20-50 cm, and the horizontal angle between the water gun and the ground is 40-60 degrees; preferably, the pressure is 150bar, the straight line distance between the gun head of the water gun and the parts is 30cm, and the horizontal angle between the water gun and the ground is 45 degrees.
In some preferred embodiments, when the parts are washed under high pressure with clear water, the water gun sprays the whole body with scattered water during spraying, and then sprays the small holes with water columns. And it should be noted that after the pressure is properly regulated, the product can be washed towards the air for several times, and after the pressure is stabilized, the product is washed at a specific angle.
In some preferred embodiments, the indoor temperature in S8 is no more than 35 ℃; preferably, the indoor temperature does not exceed 30 ℃.
In some preferred embodiments, the resistivity of water in S9 is ≡3mΩ; preferably not less than 4 M.OMEGA.
Through utilizing the nitrogen gun to weather in this application, can avoid the oxidation on dustless indoor metal surface and the attachment of dust, then can increase the air blowing volume according to actual demand to blind hole, gap, screw thread department, if when spare part surface has the dirt, then can clean with dustless cloth and electronic grade IPA and get rid of, avoid spare part after the washing to cause secondary pollution.
According to the invention, the parameter setting during the drying treatment is determined according to the complexity of the parts, and the drying time can be properly increased for the more complex parts.
In some preferred embodiments, the nitrogen flow of the oven filled with nitrogen in the step S11 is set to be 30-40L/min, the temperature is 70-80 ℃, and the time is 25-35 min; preferably, the nitrogen flow rate of the oven filled with nitrogen in the step S11 is set to be 37L/min, the temperature is 75 ℃, and the time is 30min.
In some preferred embodiments, the packaging bag in S12 is selected from one of dust-free cloth and PE bag.
And the S1-S12 are all required to be started with air stirring, and the reaction and the treatment are carried out under the stirring state. The fluidity of the treatment liquid medicine and the uniformity of the bath liquid are ensured by stirring, and further deep cleaning and reaction of parts, such as surfaces, pores and the like are promoted, so that residual metal ions of the finally cleaned aluminum alloy parts are less, and the subsequent service performance is not influenced.
In some preferred embodiments, the operations S5-S12 are all performed in a clean room not lower than Class 1000, and multiple layers of nitrile gloves are needed during the operation.
In some preferred embodiments, the nitric acid described herein is GR grade, FW 63.01; the hydrofluoric acid is of MOS grade, FW49.
The second aspect of the invention provides an application of the ultra-high clean cleaning process for the aluminum alloy parts of the semiconductor equipment in the cleaning of the aluminum alloy parts of the semiconductor equipment in the 5-nanometer process.
Compared with the prior art, the invention has the following beneficial effects:
(1) In this application with aluminum alloy spare part through in the washing liquid, acid etching solution, pickling solution, nitric acid aqueous solution soak the back, continue with high-pressure water washing, hot water washing, overflow hot water soaking, nitrogen gas weathers, toasts etc. handle, can realize fine clean effect with aluminum alloy spare part, make the spare part surface that obtains bright, the color and luster homogeneous, no spot, the mar, and the ion that obtains spare part surface residue, organic matter content are few moreover, can reach the washing standard.
(2) In the application, the nitric acid aqueous solution treatment and the subsequent operation are carried out in a dust-free room not lower than Class 1000, so that the dust-free environment is well satisfied, the reagent with a specific purity level is selected, the secondary pollution to the surface of the part after the cleaning is well avoided, and the cleaning method can be well used for cleaning the aluminum alloy part of the semiconductor equipment in a 5-nanometer process.
Detailed Description
Example 1
1. An ultra-high clean cleaning process for aluminum alloy parts of semiconductor equipment, comprising the following steps:
s1, placing a part to be cleaned in an ultrasonic cleaner containing cleaning liquid, heating to 58 ℃, cleaning for 5min, and removing oil stains on the surface of the product;
s2, placing the parts obtained after the treatment in the S1 into clean water for first filtering and cleaning to remove residual liquid medicine on the surfaces of the parts;
s3, immersing the parts obtained after the cleaning in the S2 into a container containing an acid etching solution, carrying out acid etching treatment for 13S, removing surface natural oxides, and repeating the step S2;
s4, immersing the parts obtained after the cleaning in the S3 in a container containing an acid washing solution for 3 minutes to remove new oxides on the surface, and repeating the step S2;
s5, immersing the parts obtained after the cleaning in the S4 in a nitric acid aqueous solution for 7min, and repeating the step S2;
s6, immersing the parts obtained after the treatment in the S5 in a nitric acid aqueous solution for 3min, and repeating the step S2;
s7, washing the parts obtained after the treatment in the S6 with clean water under high pressure, and further removing the liquid medicine attached to the surfaces of the products;
s8, placing the parts obtained after the cleaning in the S7 into an ultrasonic hot water tank with the temperature of 25 ℃ for filtering and cleaning for 3min;
s9, overflowing and opening 1/3, and soaking the parts obtained after the S8 cleaning with hot water at 45 ℃ for 4min;
s10, drying the parts obtained after the S9 cleaning by adopting nitrogen filtered by a 0.1 mu m filter;
s11, baking the parts obtained after the step S10 is dried in a baking oven filled with nitrogen;
and S12, vacuumizing and packaging the parts obtained after the baking in the step S11 by using dust-free cloth and packaging bags.
The cleaning solution in the step S1 is an aqueous solution containing a cleaning agent and an active agent.
The concentration of the cleaning agent is 35g/L, and the mass and volume percentage concentration of the active agent is 8.5%.
The cleaning agent is a combination of sodium phosphate, borax, sodium carbonate and polyoxyethylene polyoxypropylene ether.
The concentration percentage of the sodium phosphate, the borax, the sodium carbonate and the polyoxyethylene polyoxypropylene ether in the cleaning agent is 4.5:2.5:2:1 (Hangzhou and rhyme technologies Co., ltd.).
The active agent is linear sodium alkylbenzenesulfonate and fatty alcohol thioether sodium.
The concentration percentage of the linear sodium alkylbenzenesulfonate and the fatty alcohol sodium sulfide in the active agent is 3:2.
the straight-chain hydrocarbon R in the straight-chain sodium alkyl benzene sulfonate is C10-C16 (CAS number: 68081-81-2).
The fatty alcohol sodium thioether has the chemical formula RO (CH) 2 CH 2 O)n-SO 3 Na, wherein n=2-3, R is C12 (CAS number: 9004-82-4).
The resistivity of the water in the S2 is more than or equal to 2MΩ, the spray washing treatment time is 90S, and the temperature is 25 ℃.
The acid etching solution in the step S3 is an aqueous solution of an acidic substance.
The acidic substances are hydrofluoric acid and nitric acid.
The mass volume percentage concentration of hydrofluoric acid in the acid etching solution is 3%.
The mass volume percentage concentration of nitric acid in the acid etching solution is 20%.
The acid washing solution in the step S4 is a combination of a nitric acid aqueous solution and an ozone aqueous solution.
And in the step S4, the mass and volume percentage concentration of nitric acid in the pickling solution is 20%, and the mass and volume percentage concentration of ozone is 5%.
And the mass and volume percentage concentration of the nitric acid in the nitric acid mixed aqueous solution in the step S5 is 20%.
And (6) the mass and volume percentage concentration of the nitric acid in the nitric acid mixed water solution in the step (S6) is 10%.
And in the step S7, the pressure of the high-pressure flushing of the clean water is 150bar, the linear distance between the gun head of the water gun and the parts is 30cm, and the horizontal angle between the water gun and the ground is 45 degrees.
When the parts are washed under high pressure by clean water, the water gun sprays the whole body by using scattered water, then sprays small holes by using water columns, washes for several times towards the air, and washes products at a specific angle after the pressure is stable.
The indoor temperature in the S8 is not more than 30 ℃.
The resistivity of the water in the S9 is more than or equal to 4MΩ.
The nitrogen flow of the oven filled with nitrogen in the step S11 is set to be 37L/min, the temperature is 75 ℃, and the time is 30min.
And the packaging bag in the step S12 is a PE bag.
And the S1-S12 are all required to be started with air stirring, and the reaction and the treatment are carried out under the stirring state.
The operations of S5-S12 are all carried out in a dust-free room not lower than Class 1000, and 2 layers of nitrile gloves are needed to be worn during operation.
Nitric acid is GR grade, FW 63.01; the hydrofluoric acid is of MOS grade, FW49.
2. An application of the ultra-high clean cleaning process of the aluminum alloy parts of the semiconductor equipment in the cleaning of the aluminum alloy parts of the semiconductor equipment in the 5 nanometer manufacturing process.
Example 2
1. An antistatic and wear-resistant hard anodizing process is different from that of the embodiment 1 in that:
s1, placing a part to be cleaned in an ultrasonic cleaner containing cleaning liquid, heating to 60 ℃, cleaning for 4min, and removing oil stains on the surface of the product;
2. an application of the ultra-high clean cleaning process of the aluminum alloy parts of the semiconductor equipment in the cleaning of the aluminum alloy parts of the semiconductor equipment in the 5 nanometer manufacturing process.
Example 3
1. An antistatic and wear-resistant hard anodizing process is different from that of the embodiment 1 in that:
s1, placing a part to be cleaned in an ultrasonic cleaner containing a cleaning agent, heating to 58 ℃, cleaning for 5min, and removing oil stains on the surface of a product;
s2, placing the parts obtained after the step S1 into clear water for first filtering and cleaning to remove residual liquid medicine on the surfaces of the parts;
s3, placing the parts obtained after the step S1 into an ultrasonic cleaner containing an active agent, heating to 58 ℃, and cleaning for 5min to remove oil stains on the surface of the product;
s4 to S13 are the same as S2 to S12 in example 1.
2. An application of the ultra-high clean cleaning process of the aluminum alloy parts of the semiconductor equipment in the cleaning of the aluminum alloy parts of the semiconductor equipment in the 5 nanometer manufacturing process.
Example 4
1. An antistatic and wear-resistant hard anodizing process is different from that of the embodiment 1 in that:
and the acid washing solution in the step S4 is a nitric acid aqueous solution.
2. An application of the ultra-high clean cleaning process of the aluminum alloy parts of the semiconductor equipment in the cleaning of the aluminum alloy parts of the semiconductor equipment in the 5 nanometer manufacturing process.
Example 5
1. An antistatic and wear-resistant hard anodizing process is different from that of the embodiment 1 in that:
and in the step S4, the mass and volume percentage concentration of nitric acid in the pickling solution is 15%, and the mass and volume percentage concentration of ozone is 10%.
2. An application of the ultra-high clean cleaning process of the aluminum alloy parts of the semiconductor equipment in the cleaning of the aluminum alloy parts of the semiconductor equipment in the 5 nanometer manufacturing process.
Example 6
1. An antistatic and wear-resistant hard anodizing process is different from that of the embodiment 1 in that:
s1, placing a part to be cleaned in an ultrasonic cleaner containing cleaning liquid, heating to 58 ℃, cleaning for 5min, and removing oil stains on the surface of the product;
s2, placing the parts obtained after the treatment in the S1 into clean water for first filtering and cleaning to remove residual liquid medicine on the surfaces of the parts;
s3, immersing the parts obtained after the cleaning in the S2 into a container containing an acid etching solution, carrying out acid etching treatment for 13S, removing surface natural oxides, and repeating the step S2;
s4, immersing the parts obtained after the cleaning in the S3 in a container containing an acid washing solution for 3 minutes to remove new oxides on the surface, and repeating the step S2;
s5, washing the parts obtained after the S4 treatment with clean water under high pressure, and further removing the liquid medicine attached to the surfaces of the products;
s6, placing the parts obtained after the cleaning in the S5 into an ultrasonic hot water tank with the temperature of 25 ℃ for filtering and cleaning for 3min;
s7, overflowing and opening 1/3, and soaking the parts obtained after the cleaning in the S6 with hot water at 45 ℃ for 4min;
s8, drying the parts obtained after the cleaning of the S7 by adopting nitrogen filtered by a 0.1 mu m filter;
s9, baking the parts obtained after the step S8 of drying in a baking oven filled with nitrogen;
and S10, vacuumizing and packaging the parts obtained after the baking in the step S9 by using dust-free cloth and packaging bags.
2. An application of the ultra-high clean cleaning process of the aluminum alloy parts of the semiconductor equipment in the cleaning of the aluminum alloy parts of the semiconductor equipment in the 5 nanometer manufacturing process.
Performance testing
Ion residual quantity: the positive and negative ion contents of the sample were detected using ion chromatography (Ion Chromatography). The test procedure was carried out in a hundred-grade clean room (the test results of the polar fine dust particles in the clean room before the operation are shown in Table 1), and the samples obtained by the ultra-high clean cleaning processes obtained in example 1 and examples 2 to 6 were placed in a PP tank containing ultrapure water and allowed to stand for 24 hours. The extract was then transferred to an ion content detector for analysis and detection, and the test results are shown in Table 2.
According to the federal standard (USA Federal Standard) 209E (1992) clean room and clean room classification by dust particle concentration, class 1000 clean rooms require no more than 1000 particles with a particle size of 0.5 μm, no more than 4 particles with a particle size of greater than 5 μm. The test results in Table 1 show that the clean room in the factory meets the 1000-level clean room standard and meets the requirement of UHV cleaning on the crystal room.
Wherein F is - 、Cl - 、NO 2 - 、Br - 、NO 3 - 、PO 4 3- 、SO 4 2- The detection limits of (C) are 1.60, 2.57, 6.61, 2.67, 0.98, 0.95 and 1.28, respectively, and the units are molecular/cm 2 On the order of 10 12 。
And (3) organic matter content test: the sample of example 1 was tested for the content of volatile organic compounds on its surface using gas chromatography-mass spectrometry. The sample was subjected to chromatographic analysis using an instrument Perkin-Elmer Turbo Matrix 650, HP 6890 GC/HP 5973 MS Detector at 200℃for one hour with a carrier gas of helium type at a flow rate of 200mL/min, and the test results are shown in Table 3 below.
Claims (5)
1. An ultra-high clean cleaning process for aluminum alloy parts of semiconductor equipment is characterized by comprising the following steps:
s1, placing a part to be cleaned in an ultrasonic cleaner containing cleaning liquid, heating to 55-65 ℃, cleaning for 2-10 min, and removing oil stains on the surface of the product;
s2, placing the parts obtained after the treatment in the S1 into clean water for first filtering and cleaning to remove residual liquid medicine on the surfaces of the parts;
s3, immersing the parts obtained after the cleaning in the S2 into a container containing an acid etching solution, performing acid etching treatment for 8-18S, removing surface natural oxides, and repeating the step S2;
s4, immersing the parts obtained after the cleaning in the S3 in a container containing an acid washing solution for 1-5 minutes, removing new oxides on the surface, and repeating the step S2;
s5, immersing the parts obtained after the cleaning in the S4 in a nitric acid mixed aqueous solution for 5-10 min, and repeating the step S2;
s6, immersing the parts obtained after the treatment in the S5 in a nitric acid aqueous solution for 1-5min, and repeating the step S2;
s7, washing the parts obtained after the treatment in the S6 with clean water under high pressure, and further removing the liquid medicine attached to the surfaces of the products;
s8, placing the parts obtained after the cleaning in the S7 into an ultrasonic hot water tank with the temperature of 20-30 ℃ for filtering and cleaning for 1-5 min;
s9, overflowing and opening 1/3, and soaking the parts obtained after the S8 cleaning with hot water at 40-46 ℃ for 2-5 min;
s10, drying the parts obtained after the S9 cleaning by adopting nitrogen filtered by a 0.1 mu m filter;
s11, baking the parts obtained after the step S10 is dried in a baking oven filled with nitrogen;
s12, vacuumizing and packaging the parts obtained after the baking in the S11 by using dust-free cloth and packaging bags;
the cleaning solution in the step S1 is an aqueous solution containing a cleaning agent and an active agent; the concentration of the cleaning agent is 20-50g/L, and the mass and volume percentage concentration of the active agent is 2-30%;
the cleaning agent is a combination of sodium phosphate, borax, sodium carbonate and polyoxyethylene polyoxypropylene ether; the concentration percentage of the sodium phosphate, the borax, the sodium carbonate and the polyoxyethylene polyoxypropylene ether in the cleaning agent is (4-5): (2-3): (1.5-2.5): 1, a step of;
the active agent is linear sodium alkylbenzenesulfonate and fatty alcohol sodium sulfide; the concentration percentage of the linear sodium alkylbenzenesulfonate and the fatty alcohol sodium sulfide in the active agent is (2.5-3.5): (1.5-2.5);
the acid etching solution in the step S3 is an aqueous solution of acidic substances, the acidic substances are hydrofluoric acid and nitric acid, the mass and volume percentage concentration of the hydrofluoric acid in the acid etching solution is 1-10%, and the mass and volume percentage concentration of the nitric acid in the acid etching solution is 10-30%;
the acid washing solution in the step S4 is a combination of a nitric acid aqueous solution and an ozone aqueous solution;
the mass and volume percentage concentration of nitric acid in the acid washing solution in the step S4 is 18-23%, and the mass and volume percentage concentration of ozone is 3-8%;
the mass and volume percentage concentration of the nitric acid in the nitric acid mixed aqueous solution in the step S5 is 10-30%;
and (2) the mass and volume percentage concentration of the nitric acid in the nitric acid aqueous solution in the step (S6) is 2-20%.
2. The ultra-high clean cleaning process for the aluminum alloy parts of the semiconductor equipment according to claim 1, wherein the pressure of the high-pressure clean water flushing in the step S7 is 50-300 bar, the straight line distance between the gun head of the water gun and the parts is 20-50 cm, and the horizontal angle between the water gun and the ground is 40-60 degrees.
3. The ultra-high clean cleaning process for the aluminum alloy parts of the semiconductor equipment according to claim 1, wherein the resistivity of the water in the S2 is more than or equal to 1MΩ, the spray cleaning treatment time is 60-120S, and the temperature is 20-30 ℃.
4. The ultra-high clean cleaning process for aluminum alloy parts of semiconductor equipment according to claim 3, wherein the nitrogen flow of the oven filled with nitrogen in the step S11 is set to be 30-40L/min, the temperature is 70-80 ℃ and the time is 25-35 min.
5. Use of an ultra-high clean cleaning process for aluminum alloy parts of semiconductor equipment according to any one of claims 1-4 in cleaning aluminum alloy parts of semiconductor equipment in a 5 nm process.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310031213.XA CN115739819B (en) | 2023-01-10 | 2023-01-10 | Ultra-high clean cleaning process and application of semiconductor device aluminum alloy parts |
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| JP3239998B2 (en) * | 1998-08-28 | 2001-12-17 | 三菱マテリアルシリコン株式会社 | Semiconductor substrate cleaning method |
| CN102251242A (en) * | 2011-07-05 | 2011-11-23 | 国电宁夏太阳能有限公司 | Method for cleaning polycrystalline silicon |
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