WO2022267916A1 - 表面活性剂及其制备方法、陶瓷件清洗方法 - Google Patents
表面活性剂及其制备方法、陶瓷件清洗方法 Download PDFInfo
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- WO2022267916A1 WO2022267916A1 PCT/CN2022/098381 CN2022098381W WO2022267916A1 WO 2022267916 A1 WO2022267916 A1 WO 2022267916A1 CN 2022098381 W CN2022098381 W CN 2022098381W WO 2022267916 A1 WO2022267916 A1 WO 2022267916A1
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- ceramic
- parts
- deionized water
- surfactant
- cleaning
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- 238000000034 method Methods 0.000 title claims abstract description 104
- 238000004140 cleaning Methods 0.000 title claims abstract description 94
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- 239000008367 deionised water Substances 0.000 claims abstract description 75
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 75
- 239000002245 particle Substances 0.000 claims abstract description 75
- 239000000243 solution Substances 0.000 claims abstract description 48
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 30
- 239000003929 acidic solution Substances 0.000 claims abstract description 29
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 28
- -1 alkyl organic compound Chemical class 0.000 claims abstract description 18
- 230000007797 corrosion Effects 0.000 claims abstract description 17
- 238000005260 corrosion Methods 0.000 claims abstract description 17
- 239000003112 inhibitor Substances 0.000 claims abstract description 15
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 229910019142 PO4 Inorganic materials 0.000 claims description 16
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 16
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 16
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 15
- 239000010452 phosphate Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 11
- 239000013527 degreasing agent Substances 0.000 claims description 10
- 238000005237 degreasing agent Methods 0.000 claims description 10
- 238000010926 purge Methods 0.000 claims description 9
- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 claims description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 8
- 150000004996 alkyl benzenes Chemical class 0.000 claims description 8
- 150000008052 alkyl sulfonates Chemical class 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 8
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- 239000004065 semiconductor Substances 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- PAZSAZYCZWMYHU-UHFFFAOYSA-N butanedioic acid;phosphoric acid Chemical compound OP(O)(O)=O.OC(=O)CCC(O)=O PAZSAZYCZWMYHU-UHFFFAOYSA-N 0.000 claims description 5
- 239000004519 grease Substances 0.000 claims description 5
- 239000013543 active substance Substances 0.000 claims 2
- 229920000642 polymer Polymers 0.000 claims 1
- 229920000388 Polyphosphate Polymers 0.000 abstract description 2
- 239000001205 polyphosphate Substances 0.000 abstract description 2
- 235000011176 polyphosphates Nutrition 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 17
- 235000021317 phosphate Nutrition 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
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- 238000010586 diagram Methods 0.000 description 2
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
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- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/02—Cleaning by the force of jets or sprays
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B13/00—Accessories or details of general applicability for machines or apparatus for cleaning
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
Definitions
- the invention relates to the technical field of semiconductor processing, in particular to a surfactant, a preparation method thereof, and a cleaning method for ceramic parts.
- Alumina ceramics is a ceramic material mainly composed of alumina (Al 2 O 3 ), which is the most stable substance among oxides. It has high temperature resistance, corrosion resistance, wear resistance, high mechanical strength, high hardness, and electrical insulation. The advantages of high and low dielectric loss make alumina ceramic materials more and more used in semiconductor devices. However, this material will inevitably produce some powdery particles on the surface during the molding process of granulation, sintering and machining. Once these particles fall on the wafer during the semiconductor manufacturing process, it may affect The result of the process, for example, the conduction of different wires, the disconnection of the same wire, the formation of holes, resulting in greater energy consumption and heat generation, etc. These particles, if not removed, can seriously impact process results and chip yields.
- the existing cleaning methods for ceramic parts generally use acidic solution, alkaline solution and deionized water to clean, because many tiny particles are hidden in the grain boundaries of ceramic parts. It is difficult for acidic and alkaline solutions and deionized water to enter this gap, so that the tiny particles cannot be effectively cleaned. It is found through detection that the number of particles per unit area falling on the wafer during the process of the ceramic parts obtained by the existing ceramic parts cleaning method is ⁇ 50ea, which is much higher than the particle index (the number of particles per unit area ⁇ 2ea).
- the present invention aims to solve at least one of the technical problems existing in the prior art, and proposes a surfactant, a preparation method thereof, and a cleaning method for ceramic parts, which can effectively remove particles on ceramic parts, especially particles hidden in ceramic parts.
- the tiny particles in the gaps between the grain boundaries can solve the problem of excessive ceramic particles and improve the chip yield.
- the present invention provides a surfactant, which is used to remove the particles on the ceramic parts
- the components of the surfactant include: deionized water, organic phosphoric acid scale and corrosion inhibitors, used to improve The first organic compound for detergency and dispersibility of the surfactant, the second organic compound for removing the surface grease of the ceramic piece, polymeric phosphate, alkyl organic compound and acidic solution.
- the deionized water is 10000 parts; the organic phosphoric acid scale and corrosion inhibitor is 9-11 parts; the first organic compound is 15-17 parts; 9-11 parts of the diorganic compound; 9-11 parts of the polymeric phosphate; 14-16 parts of the alkyl organic compound; 9-11 parts of the acidic solution.
- the organic phosphoric acid scale and corrosion inhibitor includes hydroxyethylidene diphosphonic acid; the first organic compound includes alkyl sulfonate; the second organic compound includes ethylene glycol monobutyl ether;
- the polymeric phosphate includes succinate phosphate; the alkyl organic compound includes sodium alkylbenzene sulfonate; and the acidic solution includes hydrogen chloride solution.
- the deionized water is 10,000 parts; the hydroxyethylidene diphosphonic acid is 10 parts; the alkylsulfonate is 15 parts; the ethylene glycol monobutyl ether 10 parts; the succinic acid ester phosphate is 10 parts; the sodium alkylbenzene sulfonate is 15 parts; the hydrogen chloride solution is 10 parts.
- the concentration of hydrogen chloride in the hydrogen chloride solution is greater than or equal to 40% and less than or equal to 60%.
- the embodiment of the present invention also provides a method for preparing a surfactant, which is used to prepare the above-mentioned surfactant provided by the embodiment of the present invention; the preparation method includes the following steps:
- step S2 also includes:
- the solution in the reaction vessel is stirred after adding each of the components and before adding the next of the components.
- the solution in the reaction vessel is stirred for a time greater than or equal to 3 minutes and less than or equal to 5 minutes.
- an automatic stirring tool is used to stir the solution in the reaction vessel, and the rotation speed of the stirring tool is greater than or equal to 3 rpm/ minutes, and less than or equal to 5 revolutions/minute.
- the temperature of the deionized water is greater than or equal to 42°C and less than or equal to 50°C.
- an embodiment of the present invention also provides a method for cleaning ceramic parts, including:
- a chemical solution is used to dissolve the particles on the ceramic parts
- the above-mentioned surfactant provided by the embodiment of the present invention is used to clean the entire surface of the ceramic part to remove tiny particles;
- ultrasonic cleaning is used to clean the ceramic parts to remove residual particles and solutions on the ceramic parts.
- the first cleaning process specifically includes the following steps:
- the second cleaning process includes:
- the ceramic piece after the first cleaning process is soaked in the surfactant, and the entire surface of the ceramic piece is wiped at least 3 times in the surfactant.
- the third cleaning process includes the following steps:
- the ceramic part includes a ceramic process kit for semiconductor equipment.
- the components of the surfactant include: deionized water, an organic phosphoric acid scale and corrosion inhibitor, used to improve the detergency of the surfactant and Dispersive first organic compound, second organic compound for removing oily dirt on the surface of ceramic parts, polymeric phosphate, alkyl organic compound and acidic solution.
- the surfactant comprising the above-mentioned components is negatively charged or anionic, thereby effectively removing particles on a ceramic part whose polarity test is positively charged; and, the surfactant comprising the above-mentioned components has fixed hydrophilic and lipophilic groups , can be aligned on the surface of the liquid (deionized water), especially can significantly reduce the surface tension of the liquid, so that the liquid can be infiltrated into the gaps between the ceramic grain boundaries to clean and remove the hidden particles in the gaps, thereby It can solve the problem that the number of ceramic particles exceeds the standard, and improve the chip yield.
- the cleaning method of the ceramic parts divides the cleaning into three cleaning processes, wherein the first cleaning process uses a chemical solution to dissolve the particles on the ceramic parts, and this process can effectively remove the larger blind particles on the surface of the ceramic parts. holes, folds and non-welding gaps; the second cleaning process uses the above-mentioned surfactant provided by the embodiment of the present invention to clean the entire surface of the ceramic part, which can effectively remove the particles hidden in the gaps between the grain boundaries of the ceramics. Tiny particles; the third cleaning process uses ultrasonic cleaning to clean the ceramic parts to remove residual particles and solutions (acidic or alkaline solutions) on the ceramic parts, so that the ceramic parts can be fully cleaned, and finally the cleaning effect can be effectively improved.
- the first cleaning process uses a chemical solution to dissolve the particles on the ceramic parts, and this process can effectively remove the larger blind particles on the surface of the ceramic parts. holes, folds and non-welding gaps
- the second cleaning process uses the above-mentioned surfactant provided by the embodiment of the present invention to clean the entire
- Fig. 1 is the flowchart of the preparation method of the surfactant provided by the second embodiment of the present invention
- Fig. 2 is the block flow chart of the method for cleaning ceramic parts provided by the third embodiment of the present invention.
- Fig. 3 is the block flow diagram of the first cleaning process that the third embodiment of the present invention adopts
- Fig. 4 is the block flow diagram of the 3rd cleaning process that the 3rd embodiment of the present invention adopts
- Fig. 5 is the scanning electron microscope picture of the ceramic part that adopts the ceramic part cleaning method in the prior art to obtain;
- Fig. 6 is a scanning electron micrograph of a ceramic part obtained by using the method for cleaning a ceramic part provided by an embodiment of the present invention.
- the surfactant provided in this embodiment is used to remove particles on ceramic parts, such as ceramic process kits used in semiconductor equipment.
- the ceramic process kit can be components made of ceramic materials such as inner liner, medium window, nozzle, screen tube, main and auxiliary medium cylinders of three-dimensional induction coil, observation window protection cylinder and the like.
- the inventors of the present application conducted a polarity test on the above-mentioned ceramic parts, and found that the microscopic appearance of the above-mentioned ceramic parts is polar molecules, and is positively charged.
- the present invention relates to the surfactants of the invention which are negatively charged or anionic surfactants.
- the components of the above-mentioned surfactant include: deionized water, organic phosphoric acid scale and corrosion inhibitor, the first organic compound used to improve the detergency and dispersibility of the surfactant, and the Secondary organic compounds of surface grease, polymeric phosphates, alkyl organic compounds and acidic solutions.
- organic phosphoric acid scale and corrosion inhibitors have a better cleaning effect when cleaning ceramic parts.
- the organic phosphoric acid scale and corrosion inhibitor preferably includes hydroxyethylidene diphosphonic acid, which has a larger dissociation constant in deionized water (that is, the polarity parameter of a solute with a certain degree of dissociation in an aqueous solution) , the cleaning effect is better.
- the first organic compound is used to improve the detergency and dispersibility of surfactant, it can adopt the organic compound that has good detergency, foam property, emulsifying power and wetting power, for example, the first organic compound preferably comprises Alkyl sulfonate, which is easily soluble in deionized water, and has good detergency and dispersibility.
- the second organic compound is used to remove the surface grease of ceramic parts, and it can adopt the organic compound solvent that can remove the surface grease of materials such as metal, fabric, glass, plastics, for example the second organic compound preferably comprises ethylene glycol monobutyl ether, it As an excellent solvent, it can effectively remove stains on non-metallic surfaces (especially ceramic surfaces).
- Polyphosphate has excellent oil solubility and can be used as a solubilizing, emulsifying and dispersing agent with excellent performance.
- the polymeric phosphate preferably comprises succinate phosphate, which has excellent emulsifying, wetting and penetrating properties.
- Alkyl organic compounds have the effects of decontamination, wetting, foaming, emulsification, and dispersing surface activity, and the alkyl organic compounds preferably include sodium alkylbenzene sulfonate.
- the acidic solution is used to soften the ceramic particles and neutralize the pH of the ceramics.
- the acidic solution can be a volatile and water-soluble strong acid solution, such as hydrogen chloride solution.
- the surfactant comprising the above-mentioned components is negatively charged or anionic, thereby effectively removing particles on a ceramic part whose polarity test is positively charged; and, the surfactant comprising the above-mentioned components has fixed hydrophilic and lipophilic groups , can be aligned on the surface of the liquid (that is, deionized water), especially can significantly reduce the surface tension of the liquid, so that the liquid can be infiltrated into the gaps between the ceramic grain boundaries to clean and remove the hidden particles in the gaps , so as to solve the problem that the number of ceramic particles exceeds the standard, and improve the chip yield.
- the liquid that is, deionized water
- deionized water is 10,000 parts; organic phosphoric acid scale and corrosion inhibitors are 9-11 parts; the first organic compound is 15-17 parts; 9-11 parts for diorganic compounds; 9-11 parts for polymeric phosphates; 14-16 parts for alkyl organic compounds; 9-11 parts for acidic solutions.
- the surfactant containing the above-mentioned components can more effectively remove the particles hidden in the gaps by using the above-mentioned parts by weight, thereby solving the problem of exceeding the standard of the number of ceramic particles and improving the chip yield.
- the components of the above-mentioned surfactant include: deionized water, hydroxyethylidene diphosphonic acid, alkyl sulfonate, ethylene glycol monobutyl ether, succinic acid ester phosphate , sodium alkylbenzene sulfonate and hydrogen chloride solution.
- surfactants containing the above components were more effective at removing particles from ceramic parts that tested positive in polarity.
- the above-mentioned deionized water is 10,000 parts; hydroxyethylidene diphosphonic acid is 10 parts; alkylsulfonate is 15 parts; ethylene glycol monobutyl 10 parts of ether; 10 parts of succinic acid ester phosphate; 15 parts of sodium alkylbenzene sulfonate; 10 parts of hydrogen chloride solution.
- the surfactant containing the above-mentioned components has a better effect of removing hidden particles in the gaps by using the above-mentioned parts by weight.
- the concentration of hydrogen chloride in the above hydrogen chloride solution is greater than or equal to 40%, and less than or equal to 60%, preferably 50%. It should be noted that the above-mentioned concentration of hydrogen chloride is an abbreviation of the concentration of hydrogen chloride.
- the preparation method of the surfactant provided in this example is used to prepare the above-mentioned surfactant provided in this example. As shown in Figure 1, the preparation method comprises the following steps:
- the temperature of the deionized water is greater than or equal to 42°C and less than or equal to 50°C.
- a temperature atmosphere conducive to the rapid dissolution of the added components can be created.
- hydroxyethylidene diphosphonic acid, alkyl sulfonate, ethylene glycol monobutyl ether, succinate phosphate , sodium alkylbenzene sulfonate, and hydrogen chloride solution are added to the reaction vessel, and the solution in the reaction vessel is stirred during the addition of each component.
- the solution in the reaction vessel is continuously stirred to accelerate the dissolution of the component.
- automatic or manual stirring tools can be used to stir the solution in the reaction vessel.
- an automatic stirring tool is used to stir the solution in the reaction vessel, and the rotation speed of the stirring tool is greater than or equal to 3 revolutions /min, and less than or equal to 5 revolutions/min. In this way, the dissolution of the components can be effectively accelerated.
- step S2 further includes:
- the solution in the reaction vessel is not only stirred during the addition of each component, but also after each component is added and before the next component is added , which can further improve the dissolution effect of the components.
- the time for stirring the solution in the reaction vessel is greater than or equal to 3 minutes and less than or equal to 5 minutes.
- the preparation method of the surfactant provided in this example is safe, efficient, simple in process, and easy to implement.
- present embodiment provides a kind of cleaning method of ceramic parts, it comprises:
- a chemical solution is used to dissolve the particles on the ceramic parts
- the first cleaning process can effectively clean the particles on the surface of the ceramic part, especially the particles in the larger blind holes, folds and non-welding gaps on the surface of the ceramic part.
- the above-mentioned surfactant provided in this embodiment is used to clean the entire surface of the ceramic part to remove tiny particles;
- the above-mentioned surfactants provided in this embodiment are negatively charged or anionic, and the polar molecules of the ceramic parts are positively charged, the above-mentioned surfactants can effectively remove particles on the ceramic parts; and, the above-mentioned surface active agents provided in this embodiment
- the agent has a fixed hydrophilic and lipophilic group, which can be aligned on the surface of the liquid, especially can significantly reduce the surface tension of the liquid, so that the liquid can be infiltrated into the gaps between the ceramic grain boundaries, so as to hide the gaps in the gaps. Particle cleaning removes, which in turn can greatly reduce the particle count.
- ultrasonic cleaning is used to clean the ceramic parts to remove residual particles and solutions on the ceramic parts.
- the so-called ultrasonic cleaning refers to the cleaning of particles on ceramic parts by water waves generated by ultrasonic vibration.
- the third cleaning process can fully clean the ceramic parts, and finally can effectively improve the cleaning effect.
- the first cleaning process specifically includes the following steps:
- Alkaline degreasers can dissolve particles on ceramic parts.
- the time for the ceramic parts to be soaked in the alkaline degreasing agent is greater than or equal to 50 minutes and less than or equal to 80 minutes.
- the above step S102 is used to clean the alkaline degreasing agent on the ceramic part, so as to prevent the alkaline degreasing agent from damaging the sealing surface and the edge of the hole of the ceramic part and affecting the sealing performance of the part.
- the above step S103 is used to further remove particles and residual solution on the ceramic piece.
- the range of the above specified pressure is greater than or equal to 40 psi and less than or equal to 60 psi.
- the above step S104 can neutralize the alkaline solution remaining on the ceramic part, so as to reduce the corrosion of the ceramic part by the alkaline solution and prevent the alkaline solution from damaging the sealing surface and the edge of the hole of the ceramic part.
- the time range for the ceramic piece to be soaked in the acidic solution is greater than or equal to 5 minutes and less than or equal to 10 minutes.
- the above-mentioned acidic solution is hydrochloric acid or fluoronitric acid solution, wherein the fluoronitric acid solution has a better dissolution effect with an alkaline solution (such as KOH solution).
- an alkaline solution such as KOH solution
- the above step S105 is used to clean the acidic solution on the ceramic piece.
- the above step S106 is used to further remove particles and residual solution on the ceramic piece.
- the range of the above specified pressure is greater than or equal to 40 psi and less than or equal to 60 psi.
- the above-mentioned second cleaning process includes:
- the ceramic piece in the process of wiping the entire surface of the ceramic piece, the ceramic piece is always soaked in the above-mentioned surfactant, which is more conducive to making the liquid infiltrate into the gap between the grain boundaries of the ceramic, so as to hide the surface in the gap.
- the particles are cleaned and removed.
- the third cleaning process specifically includes the following steps:
- the range of the resistivity of the deionized water is greater than or equal to 2 M ⁇ cm, and the range of the cleaning time is greater than or equal to 10 minutes and less than or equal to 15 minutes.
- the above step S301 can fully clean the ceramic parts. Since the cleaning effect of ultrasonic cleaning with deionized water is the most obvious, after the ultrasonic cleaning step is completed, the cleaning effect of the ceramic parts can be guaranteed to meet the process requirements. Moreover, the removal of the particles on the surface of the ceramic piece and the tiny particles in the gaps between the ceramic grain boundaries has been achieved by using the previous first cleaning process and the second cleaning process, so that they cannot be removed before ultrasonic cleaning particles are removed.
- the resistivity of the deionized water used in the above step S302 is higher than the resistivity of the deionized water used in the above step S301, for example, in the above step S301, the range of the resistivity of the deionized water is greater than or equal to 2M ⁇ cm, and In the above step S302, the range of the resistivity of the deionized water is greater than or equal to 4M ⁇ cm.
- the temperature of the deionized water used in the above step S302 is higher than the temperature of the deionized water used in the above step S301.
- the temperature of the deionized water used in the above step S302 is normal temperature (generally 25°C), while the temperature range of the deionized water used in the above step S301 is greater than or equal to 32°C and less than or equal to 42°C.
- new deionized water is always introduced into the cleaning tank, and the deionized water in the cleaning tank is discharged by overflow, so that the deionized water can be in circulation flow state, which can further improve the cleaning effect.
- the purging gas used in the above step S303 includes nitrogen, the purity of which is 99.999%; the range of the included angle between the purging direction of nitrogen and the surface of the ceramic part is, for example, greater than or equal to 30°, and less than or equal to 45° ° to avoid re-falling of particles on the surface of ceramic parts.
- the flow process of the cleaning method for ceramic parts in the prior art is as follows: first, soak the ceramic parts in an alkaline degreasing agent for 50min-80min, then put the ceramic parts into deionized water for rinsing (using pressurized deionized water to spray all over the surface of the ceramic piece); after that, immerse the ceramic piece in the acidic solution for 5min-10min, then take the ceramic piece out of the solution, and immerse it in deionized water again for the above rinsing, and then immerse the resistivity greater than or equal to 4M ⁇ cm 1.
- Ultrasonic cleaning in deionized water at room temperature for 10min-15min then immerse the ceramic parts in deionized water with a resistivity greater than or equal to 8M ⁇ cm for hot water immersion, and finally use nitrogen to dry the ceramic parts and dry the ceramic parts to complete the entire cleaning process.
- the ceramic parts cleaning method provided by the embodiment of the present invention includes the above three cleaning processes, wherein the first cleaning process includes the above steps S101-S106; the second cleaning process includes soaking the sprayed ceramic parts in the above surfactant, And wipe the entire surface of the ceramic piece in the surfactant for at least 3 times; the third cleaning process includes the above steps S301-S303.
- Fig. 5 is a scanning electron microscope image of a ceramic part obtained by using the cleaning method of the ceramic part in the prior art.
- Fig. 6 is a scanning electron micrograph of a ceramic part obtained by using the method for cleaning a ceramic part provided by an embodiment of the present invention. Comparing Fig. 5 and Fig. 6, it can be seen that the ceramic part obtained by the ceramic part cleaning method in the prior art still has suspended particles on its surface, and (a) figure in Fig. 5 is an electron microscope after the surface of the ceramic part is magnified 2000 times Scanning picture; (b) picture is the scanning electron microscope picture after magnifying 5000 times to the surface of ceramic piece; As shown in (a) picture and (b) picture among Fig. 5, the white dot on the black region in the figure is for suspended particles.
- the ceramic part in this embodiment includes, for example, a ceramic process kit for semiconductor equipment.
- the ceramic process kit can be components made of ceramic materials such as inner liner, medium window, nozzle, screen tube, main and auxiliary medium cylinders of three-dimensional induction coil, observation window protection cylinder and the like.
- the method for cleaning ceramic parts divides the cleaning into three cleaning processes, wherein the first cleaning process uses a chemical solution to dissolve the particles on the ceramic parts, and this process can effectively reduce the size of the ceramic parts on the surface. Larger blind holes, wrinkles and non-welding gaps are cleaned; the second cleaning process uses the above-mentioned surfactant provided in this embodiment to clean the entire surface of the ceramic part, which can effectively remove the particles hidden between the grain boundaries of the ceramic. Tiny particles in the gaps; the third cleaning process uses ultrasonic cleaning to clean the ceramic parts to remove the remaining particles and solutions (acidic or alkaline solutions) on the ceramic parts, so that the ceramic parts can be fully cleaned, and finally can be effectively improved. cleaning effect.
- the first cleaning process uses a chemical solution to dissolve the particles on the ceramic parts, and this process can effectively reduce the size of the ceramic parts on the surface. Larger blind holes, wrinkles and non-welding gaps are cleaned; the second cleaning process uses the above-mentioned surfactant provided in this embodiment to clean the entire surface of the ceramic
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Abstract
本发明实施例提供一种表面活性剂及其制备方法、陶瓷件清洗方法，该表面活性剂，用于去除陶瓷件上的颗粒，表面活性剂的组分包括：去离子水、有机磷酸类阻垢缓蚀剂、用于提高表面活性剂的去污力和分散性的第一有机化合物、用于去除陶瓷件的表面油垢的第二有机化合物、聚合磷酸盐、烷基类有机化合物以及酸性溶液。本发明实施例提供的表面活性剂及其制备方法、陶瓷件清洗方法的技术方案，可以有效去除陶瓷件上的颗粒，尤其是隐藏在陶瓷的晶界之间的缝隙中的微小颗粒，从而可以解决陶瓷颗粒数量超标的问题，提高芯片良率。
Description
本发明涉及半导体加工技术领域，具体地，涉及一种表面活性剂及其制备方法、陶瓷件清洗方法。
在集成电路的制造过程中，污染是个不可忽视的因素，据统计，有50％的良率损失来源于污染，而颗粒污染又是主要污染源之一。颗粒在附着于晶圆表面时，在膜层沉积的过程中可能成为掩埋缺陷，在刻蚀的过程中可能阻断光刻图案向膜层图案的转移，在制程的后段部分，还可能引起导线的断开和临近接线的导通。一般情况下，颗粒尺寸如果超过器件最小特征尺寸的50％，就有导致器件失效的可能。因此，随着集成电路微型化需求的持续及工艺难度的提高，对颗粒污染的控制是保证生产效率及产品良率的一条必要条件。
氧化铝陶瓷是一种以氧化铝(Al
2O
3)为主体的陶瓷材料，是氧化物中最稳定的物质，具有耐高温、耐腐蚀、耐磨、机械强度高、硬度大、电绝缘性高与介电损耗低等的优势，这使得氧化铝陶瓷材料越来越多地应用在半导体设备中。但是，这种材料在造粒、烧结和机加工等的成型过程中不可避免地会在表面产生一些粉末状的颗粒，这些颗粒一旦在半导体制备工艺过程中掉落在晶圆上，可能会影响工艺结果，例如，不同导线的导通、同一导线的断连、形成空穴而造成更大能耗和发热等。这些颗粒如果不加以去除，会严重影响到工艺结果和芯片良率。
为了去除陶瓷件上的颗粒，就需要对陶瓷件进行清洗，但是，现有的陶 瓷件清洗方法一般采用酸性溶液、碱性溶液及去离子水清洗，由于许多微小颗粒隐藏在陶瓷件的晶界之间的缝隙，而酸性、碱性溶液及去离子水很难进入到这个缝隙，从而无法对微小颗粒进行有效清洗。通过检测发现，采用现有的陶瓷件清洗方法获得的陶瓷件，其在工艺过程中落在晶圆上的每单位面积的颗粒数量≥50ea，远高于颗粒指标(每单位面积的颗粒数量<2ea)。
发明内容
本发明旨在至少解决现有技术中存在的技术问题之一，提出了一种表面活性剂及其制备方法、陶瓷件清洗方法，其可以有效去除陶瓷件上的颗粒，尤其是隐藏在陶瓷的晶界之间的缝隙中的微小颗粒，从而可以解决陶瓷颗粒数量超标的问题，提高芯片良率。
为实现上述目的，本发明提供了一种表面活性剂，用于去除陶瓷件上的颗粒，所述表面活性剂的组分包括：去离子水、有机磷酸类阻垢缓蚀剂、用于提高所述表面活性剂的去污力和分散性的第一有机化合物、用于去除所述陶瓷件的表面油垢的第二有机化合物、聚合磷酸盐、烷基类有机化合物以及酸性溶液。
可选的，按重量份数计，所述去离子水为10000份；所述有机磷酸类阻垢缓蚀剂为9-11份；所述第一有机化合物为15-17份；所述第二有机化合物为9-11份；所述聚合磷酸盐为9-11份；所述烷基类有机化合物为14-16份；所述酸性溶液为9-11份。
可选的，所述有机磷酸类阻垢缓蚀剂包括羟基乙叉二膦酸；所述第一有机化合物包括烷基磺酸盐；所述第二有机化合物包括乙二醇单丁醚；所述聚合磷酸盐包括琥珀酸脂磷酸盐；所述烷基类有机化合物包括烷基苯磺酸钠；所述酸性溶液包括氯化氢溶液。
可选的，按重量份数计，所述去离子水为10000份；所述羟基乙叉二膦酸为10份；所述烷基磺酸盐为15份；所述乙二醇单丁醚为10份；所述琥珀 酸脂磷酸盐为10份；所述烷基苯磺酸钠为15份；所述氯化氢溶液为10份。
可选的，所述氯化氢溶液中氯化氢的浓度大于等于40％，且小于等于60％。
作为另一个技术方案，本发明实施例还提供一种表面活性剂的制备方法，用于制备本发明实施例提供的上述表面活性剂；所述制备方法包括以下步骤：
S1、将所述去离子水加入反应容器中；
S2、按时间的先后顺序依次将所述有机磷酸类阻垢缓蚀剂、所述第一有机化合物、所述第二有机化合物、所述聚合磷酸盐、所述烷基类有机化合物以及所述酸性溶液加入所述反应容器中，并在加入每个所述组分的过程中对所述反应容器中的溶液进行搅拌。
可选的，所述步骤S2，还包括：
在加入每个所述组分之后，且在加入下一个所述组分之前，对所述反应容器中的溶液进行搅拌。
可选的，在加入每个所述组分之后，且在加入下一个所述组分之前，对所述反应容器中的溶液进行搅拌的时间大于等于3min，且小于等于5min。
可选的，所述步骤S2中，在加入每个所述组分的过程中，使用自动的搅拌工具对所述反应容器中的溶液进行搅拌，且所述搅拌工具的转速大于等于3转/分钟，且小于等于5转/分钟。
可选的，在所述步骤S1中，所述去离子水的温度大于等于42℃，且小于等于50℃。
作为另一个技术方案，本发明实施例还提供一种陶瓷件清洗方法，包括：
第一清洗过程，采用化学溶液溶解陶瓷件上的颗粒；
第二清洗过程，采用本发明实施例提供的上述表面活性剂清洗所述陶瓷件的整个表面，以去除微小颗粒；
第三清洗过程，采用超声波清洗的方式清洗所述陶瓷件，以去除所述陶瓷件上残留的颗粒和溶液。
可选的，所述第一清洗过程具体包括以下步骤：
S101、将陶瓷件浸泡在碱性脱脂剂中；
S102、将在所述碱性脱脂剂中浸泡后的所述陶瓷件浸泡在去离子水中；
S103、使用指定压力的去离子水喷淋在所述去离子水中浸泡后的所述陶瓷件的整个表面；
S104、将喷淋后的所述陶瓷件浸泡在酸性溶液中；
S105、将浸泡在所述酸性溶液中的所述陶瓷件浸泡在去离子水中；
S106、使用所述指定压力的去离子水喷淋在所述去离子水中浸泡后的所述陶瓷件的整个表面。
可选的，所述第二清洗过程包括：
将完成所述第一清洗过程的所述陶瓷件浸泡在所述表面活性剂中，并在所述表面活性剂中擦拭所述陶瓷件的整个表面至少3次。
可选的，所述第三清洗过程包括以下步骤：
S301、将完成所述第二清洗过程的所述陶瓷件浸泡在去离子水中，并进行超声波清洗；
S302、将超声波清洗后的所述陶瓷件浸泡在去离子水中，其中，所述步骤S302采用的去离子水的电阻率高于所述步骤S301采用的去离子水的电阻率；所述步骤S302采用的去离子水的温度高于所述步骤S301采用的去离子水的温度；
S303、对清洗后的所述陶瓷件进行吹扫，并在吹扫后对所述陶瓷件进行烘烤。
可选的，所述陶瓷件包括用于半导体设备的陶瓷工艺套件。
本发明的有益效果：
本发明实施例提供的表面活性剂及其制备方法的技术方案中，表面活性剂的组分包括：去离子水、有机磷酸类阻垢缓蚀剂、用于提高表面活性剂的去污力和分散性的第一有机化合物、用于去除陶瓷件的表面油垢的第二有机化合物、聚合磷酸盐、烷基类有机化合物以及酸性溶液。包含上述组分的表面活性剂带负电或者阴离子，从而可以有效去除极性测试为带正电的陶瓷件上的颗粒；并且，包含上述组分的表面活性剂具有固定的亲水亲油基团，能够在液体(去离子水)表面定向排列，特别是能够使液体表面张力显著降低，从而可以使液体浸润到陶瓷晶界之间的缝隙中，以将该缝隙中隐藏的颗粒清洗去除，从而可以解决陶瓷颗粒数量超标的问题，提高芯片良率。
本发明实施例提供的陶瓷件清洗方法，将清洗分为三个清洗过程，其中，第一清洗过程采用化学溶液溶解陶瓷件上的颗粒，该过程可以有效对陶瓷件表面上尺寸较大的盲孔、褶皱及非焊接缝隙处的颗粒进行清洗；第二清洗过程采用本发明实施例提供的上述表面活性剂清洗陶瓷件的整个表面，可以有效去除隐藏在陶瓷的晶界之间的缝隙中的微小颗粒；第三清洗过程采用超声波清洗的方式清洗陶瓷件，以去除陶瓷件上残留的颗粒和溶液(酸性或碱性溶液)，从而可以对陶瓷件进行全面清洗，最终可以有效提高清洗效果。
图1为本发明第二实施例提供的表面活性剂的制备方法的流程框图；
图2为本发明第三实施例提供的陶瓷件清洗方法的流程框图；
图3为本发明第三实施例采用的第一清洗过程的流程框图；
图4为本发明第三实施例采用的第三清洗过程的流程框图；
图5为采用现有技术中的陶瓷件清洗方法获得的陶瓷件的电镜扫描图；
图6为采用本发明实施例提供的陶瓷件清洗方法获得的陶瓷件的电镜扫描图。
为使本领域的技术人员更好地理解本发明的技术方案，下面结合附图对本发明实施例提供的表面活性剂及其制备方法、陶瓷件清洗方法进行详细描述。
第一实施例
本实施例提供的表面活性剂，用于去除陶瓷件上的颗粒，该陶瓷件例如包括用于半导体设备的陶瓷工艺套件。该陶瓷工艺套件可以是诸如内衬、介质窗、喷嘴、筛管、立体感应线圈的主、副介质筒、观察窗保护筒等采用陶瓷材料制备的部件。
本申请发明人对上述陶瓷件进行极性测试，发现上述陶瓷件微观表现为极性分子，且带正电。本发明涉及发明的表面活性剂属于负电或者阴离子表面活性剂。
具体地，上述表面活性剂的组分包括：去离子水、有机磷酸类阻垢缓蚀剂、用于提高表面活性剂的去污力和分散性的第一有机化合物、用于去除陶瓷件的表面油垢的第二有机化合物、聚合磷酸盐、烷基类有机化合物以及酸性溶液。
其中，有机磷酸类阻垢缓蚀剂对陶瓷件进行清洗时具有较佳的清洗效果。可选的，该有机磷酸类阻垢缓蚀剂优选包括羟基乙叉二膦酸，其在去离子水中具有较大的离解常数(即，水溶液中具有一定解离度的溶质的极性参数)，清洗效果更佳。
第一有机化合物用于提高表面活性剂的去污力和分散性，其可以采用具有较好的去污力、泡沫性、乳化力和润湿力的有机化合物，例如，第一有机化合物优选包括烷基磺酸盐，其易溶于去离子水，且具有良好的去污力和分散性。
第二有机化合物用于去除陶瓷件的表面油垢，其可以采用可清除金属、 织物、玻璃、塑料等材料的表面油垢的有机化合物溶剂，例如第二有机化合物优选包括乙二醇单丁醚，其可作为优良溶剂，可以有效清除非金属表面(尤其是陶瓷表面)的污渍。
聚合磷酸盐具有优异的油溶性，可以作为性能极佳的增溶、乳化和分散剂。该聚合磷酸盐优选包括琥珀酸脂磷酸盐，其具有优异的乳化、润湿和渗透等性能。
烷基类有机化合物具有去污、湿润、发泡、乳化、分散的表面活性等作用，该烷基类有机化合物优选包括烷基苯磺酸钠。
酸性溶液用于软化陶瓷颗粒、中和陶瓷的酸碱度，该酸性溶液可以采用易挥发、易溶于水的强酸溶液，例如氯化氢溶液。
包含上述组分的表面活性剂带负电或者阴离子，从而可以有效去除极性测试为带正电的陶瓷件上的颗粒；并且，包含上述组分的表面活性剂具有固定的亲水亲油基团，能够在液体(即，去离子水)表面定向排列，特别是能够使液体表面张力显著降低，从而可以使液体浸润到陶瓷晶界之间的缝隙中，以将该缝隙中隐藏的颗粒清洗去除，从而可以解决陶瓷颗粒数量超标的问题，提高芯片良率。
在一些优选的实施例中，可选的，按重量份数计，去离子水为10000份；有机磷酸类阻垢缓蚀剂为9-11份；第一有机化合物为15-17份；第二有机化合物为9-11份；聚合磷酸盐为9-11份；烷基类有机化合物为14-16份；酸性溶液为9-11份。包含上述组分的表面活性剂通过采用上述重量份数，可以更有效地将缝隙中隐藏的颗粒去除，从而可以解决陶瓷颗粒数量超标的问题，提高芯片良率。
在一些优选的实施例中，可选的，上述表面活性剂的组分包括：去离子水、羟基乙叉二膦酸、烷基磺酸盐、乙二醇单丁醚、琥珀酸脂磷酸盐、烷基苯磺酸钠以及氯化氢溶液。包含上述组分的表面活性剂去除极性测试为带正 电的陶瓷件上的颗粒的效果更佳。
在一些优选的实施例中，可选的，按重量份数计，上述去离子水为10000份；羟基乙叉二膦酸为10份；烷基磺酸盐为15份；乙二醇单丁醚为10份；琥珀酸脂磷酸盐为10份；烷基苯磺酸钠为15份；氯化氢溶液为10份。包含上述组分的表面活性剂通过采用上述重量份数，去除缝隙中隐藏的颗粒的效果更佳。
在一些优选的实施例中，可选的，上述氯化氢溶液中氯化氢的浓度为大于等于40％，且小于等于60％，优选为50％。需要说明的是，上述氯化氢的浓度是氯化氢的量浓度的简称。
第二实施例
本实施例提供的表面活性剂的制备方法，用于制备本实施例提供的上述表面活性剂。如图1所示，该制备方法包括以下步骤：
S1、将去离子水加入反应容器中；
可选的，在上述步骤S1中，去离子水的温度大于等于42℃，且小于等于50℃。通过将去离子水的温度设定在该范围内，可以制造出有利于加入的组分迅速溶解的温度氛围。
S2、按时间的先后顺序依次将有机磷酸类阻垢缓蚀剂、第一有机化合物、第二有机化合物、聚合磷酸盐、烷基类有机化合物以及酸性溶液加入反应容器中，并在加入每个组分的过程中对反应容器中的溶液进行搅拌，即，一边加入组分一边进行搅拌。
在一些优选的实施例中，可选的，在上述步骤S2中，按时间的先后顺序依次将羟基乙叉二膦酸、烷基磺酸盐、乙二醇单丁醚、琥珀酸脂磷酸盐、烷基苯磺酸钠以及氯化氢溶液加入反应容器中，并在加入每个组分的过程中对反应容器中的溶液进行搅拌。
具体来说，在每加入一种组分的过程中，持续对反应容器中的溶液进行 搅拌，以加速组分的溶解。在实际应用中，可以使用自动或者手动的搅拌工具对反应容器中的溶液进行搅拌。
在一些优选的实施例中，可选的，上述步骤S2中，在加入每个组分的过程中，使用自动的搅拌工具对反应容器中的溶液进行搅拌，且搅拌工具的转速大于等于3转/分钟，且小于等于5转/分钟。这样，可以有效加速组分的溶解。
在一些优选的实施例中，可选的，上述步骤S2，还包括：
在加入每个组分之后，对反应容器中的溶液进行搅拌。
也就是说，不仅在加入每个组分的过程中对反应容器中的溶液进行搅拌，在每个组分加入之后，且在加入下一个组分之前，也要对反应容器中的溶液进行搅拌，这样可以进一步提高组分的溶解效果。
可选的，在每个组分加入之后，且在加入下一个组分之前，对反应容器中的溶液进行搅拌的时间大于等于3min，且小于等于5min。
在最后一个组分加入反应容器中，并完成相应的搅拌之后，即可获得本实施例提供的上述表面活性剂。
本实施例提供的表面活性剂的制备方法，其安全高效、工艺精简，且易于实现。
第三实施例
请参阅图2，本实施例提供一种陶瓷件清洗方法，其包括：
第一清洗过程，采用化学溶液溶解陶瓷件上的颗粒；
第一清洗过程可以有效对陶瓷件表面上的颗粒进行清洗，尤其是陶瓷件表面上尺寸较大的盲孔、褶皱及非焊接缝隙处的颗粒进行清洗。
第二清洗过程，采用本实施例提供的上述表面活性剂清洗所述陶瓷件的整个表面，以去除微小颗粒；
由于本实施例提供的上述表面活性剂带负电或者阴离子，而陶瓷件的极 性分子带正电，从而上述表面活性剂可以有效去除陶瓷件上的颗粒；并且，本实施例提供的上述表面活性剂具有固定的亲水亲油基团，能够在液体表面定向排列，特别是能够使液体表面张力显著降低，从而可以使液体浸润到陶瓷晶界之间的缝隙中，以将该缝隙中隐藏的颗粒清洗去除，进而可以大大减少颗粒数量。
第三清洗过程，采用超声波清洗的方式清洗陶瓷件，以去除陶瓷件上残留的颗粒和溶液。
所谓超声波清洗，是指通过超声波震荡产生的水波清洗陶瓷件上的颗粒。第三清洗过程可以对陶瓷件进行全面清洗，最终可以有效提高清洗效果。
下面对上述第一清洗过程的具体实施方式进行详细描述。具体地，如图3所示，第一清洗过程具体包括以下步骤：
S101、将陶瓷件浸泡在碱性脱脂剂中；
碱性脱脂剂可以溶解陶瓷件上的颗粒。
为了有效溶解陶瓷件上的颗粒，提高清洗效果，可选的，上述步骤S101中，陶瓷件浸泡在碱性脱脂剂中的时间的范围为大于等于50min，且小于等于80min。
S102、将在碱性脱脂剂中浸泡后的陶瓷件浸泡在去离子水中；
上述步骤S102用于清洗陶瓷件上的碱性脱脂剂，避免碱性脱脂剂对陶瓷件的密封面和孔边缘处产生损伤，影响零件的密封性。
S103、使用指定压力的去离子水喷淋在去离子水中浸泡后的陶瓷件的整个表面；
上述步骤S103用于进一步去除陶瓷件上的颗粒和残留溶液。
为了进一步提高清洗效果，可选的，上述指定压力的范围为大于等于40psi，且小于等于60psi。
S104、将喷淋后的陶瓷件浸泡在酸性溶液中；
上述步骤S104可以中和残留在陶瓷件上的碱性溶液，以减少碱性溶液对陶瓷件的腐蚀，避免碱性溶液对陶瓷件的密封面和孔边缘处产生损伤。
可选的，上述步骤S104中，陶瓷件浸泡在酸性溶液中的时间的范围为大于等于5min，且小于等于10min。
可选的，上述酸性溶液为盐酸或者氟硝酸溶液，其中，氟硝酸溶液与碱性溶液(例如KOH溶液)的溶解作用更优。
S105、将浸泡在酸性溶液中的陶瓷件浸泡在去离子水中；
上述步骤S105用于清洗陶瓷件上的酸性溶液。
S106、使用上述指定压力的去离子水喷淋在去离子水中浸泡后的陶瓷件的整个表面。
上述步骤S106用于进一步去除陶瓷件上的颗粒和残留溶液。
为了进一步提高清洗效果，可选的，上述指定压力的范围为大于等于40psi，且小于等于60psi。
可选的，上述第二清洗过程包括：
将完成上述第一清洗过程的陶瓷件浸泡在上述表面活性剂中，并在该表面活性剂中擦拭陶瓷件的整个表面至少3次。
也就是说，在擦拭陶瓷件的整个表面的过程中，该陶瓷件始终浸泡在上述表面活性剂中，这样更有利于使液体浸润到陶瓷晶界之间的缝隙中，以将该缝隙中隐藏的颗粒清洗去除。
需要说明的是，将陶瓷件浸泡在上述表面活性剂中，擦拭陶瓷件直至整个表面均被擦拭，该过程为第1次；然后重新将陶瓷件浸泡在未使用的表面活性剂中，并擦拭陶瓷件直至整个表面均被擦拭，该过程为第2次，以此类推。
下面对上述第三清洗过程的具体实施方式进行详细描述。具体地，如图4所示，第三清洗过程具体包括以下步骤：
S301、将完成上述第二清洗过程的陶瓷件浸泡在去离子水中，并进行超声波清洗；
可选的，上述步骤S301中，去离子水的电阻率的范围为大于等于2MΩ·cm，且清洗时间的范围为大于等于10min，且小于等于15min。
上述步骤S301可以对陶瓷件进行全面清洗，由于使用去离子水进行超声波清洗的清洗效果最明显，在完成超声波清洗步骤之后，可以保证陶瓷件的清洗效果满足工艺要求。而且，利用前面的第一清洗过程和第二清洗过程已经实现了陶瓷件表面上的颗粒以及陶瓷晶界之间的缝隙中的微小颗粒的去除，从而可以在进行超声波清洗之前，将其无法去除的颗粒进行去除。
S302、将超声波清洗后的陶瓷件浸泡在去离子水中；
其中，上述步骤S302采用的去离子水的电阻率高于上述步骤S301采用的去离子水的电阻率，例如，上述步骤S301中，去离子水的电阻率的范围为大于等于2MΩ·cm，而上述步骤S302中，上述去离子水的电阻率的范围为大于等于4MΩ·cm。
上述步骤S302采用的去离子水的温度高于上述步骤S301采用的去离子水的温度。例如，上述步骤S302采用的去离子水的温度为常温(一般为25℃)，而上述步骤S301采用的去离子水的温度的范围为大于等于32℃，且小于等于42℃。
为了提高清洗效果，可选的，在浸泡过程中，始终向清洗槽中通入新的去离子水，并采用溢流的方式排出该清洗槽中的去离子水，可以使去离子水处于循环流动状态，从而可以进一步提高清洗效果。
S303、对浸泡后的陶瓷件进行吹扫，并在吹扫后对陶瓷件进行烘烤。
可选的，上述步骤S303采用的吹扫气体包括氮气，该氮气的纯度为99.999％；氮气的吹扫方向与陶瓷件表面之间的夹角的范围例如为大于等于30°，且小于等于45°，以避免颗粒重新掉落在陶瓷件表面。
可选的，首先使用干燥氮气对陶瓷件进行全面吹扫；然后使用干燥氮气吹扫净化炉(或烘箱)，以烘干其内部；最后，将陶瓷件放入吹扫后的净化炉(或烘箱)中进行烘烤。
下面将采用现有技术中的陶瓷件清洗方法和本发明实施例提供的陶瓷件清洗方法分别获得的陶瓷件进行对比实验。具体地，现有技术中的陶瓷件清洗方法的流程为：首先将陶瓷件浸入碱性脱脂剂中浸泡50min-80min，再将陶瓷件放入去离子水中漂洗(使用加压去离子水喷淋陶瓷件表面各处)；之后，将陶瓷件浸入酸性溶液中浸泡5min-10min，然后将陶瓷件从溶液中取出，并再次浸入去离子水中进行上述漂洗，之后浸入电阻率率大于等于4MΩ·cm、常温的去离子水中进行超声波清洗10min-15min，之后将陶瓷件浸入电阻率大于等于8MΩ·cm的去离子水中进行热水浸洗，最后使用氮气吹干陶瓷件，并烘干陶瓷件，完成整个清洗流程。
本发明实施例提供的陶瓷件清洗方法包括上述三个清洗过程，其中，第一清洗过程包括上述步骤S101-S106；第二清洗过程包括将喷淋后的陶瓷件浸泡在上述表面活性剂中，并在该表面活性剂中擦拭陶瓷件的整个表面至少3次；第三清洗过程包括上述步骤S301-S303。
图5为采用现有技术中的陶瓷件清洗方法获得的陶瓷件的电镜扫描图。图6为采用本发明实施例提供的陶瓷件清洗方法获得的陶瓷件的电镜扫描图。对比图5和图6可知，采用现有技术中的陶瓷件清洗方法获得的陶瓷件，其表面仍然存在悬浮颗粒，图5中的(a)图为对陶瓷件的表面放大2000倍后的电镜扫描图；(b)图为对陶瓷件的表面放大5000倍后的电镜扫描图；如图5中的(a)图和(b)图所示，图中黑色区域上的白色点状物即为悬浮颗粒。此外，现有技术中的陶瓷件清洗方法获得的陶瓷件，其在工艺过程中落在晶圆上的每单位面积的颗粒数量≥50ea，远高于颗粒指标(每单位面积的颗粒数量<2ea)。与之相比，图6中的(a)图为对陶瓷件的表面放大2000 倍后的电镜扫描图；(6)图为对陶瓷件的表面放大5000倍后的电镜扫描图；如图6中的(a)图和(b)图所示，图中黑色区域上的白色点状物显著减少，由此可知，采用本发明实施例提供的陶瓷件清洗方法获得的陶瓷件上的悬浮颗粒显著减少，该陶瓷件在工艺过程中落在晶圆上的每单位面积的颗粒数量低于颗粒指标(每单位面积的颗粒数量<2ea)。
本实施例中的陶瓷件例如包括用于半导体设备的陶瓷工艺套件。该陶瓷工艺套件可以是诸如内衬、介质窗、喷嘴、筛管、立体感应线圈的主、副介质筒、观察窗保护筒等采用陶瓷材料制备的部件。
综上所述，本实施例提供的陶瓷件清洗方法，将清洗分为三个清洗过程，其中，第一清洗过程采用化学溶液溶解陶瓷件上的颗粒，该过程可以有效对陶瓷件表面上尺寸较大的盲孔、褶皱及非焊接缝隙处的颗粒进行清洗；第二清洗过程采用本实施例提供的上述表面活性剂清洗陶瓷件的整个表面，可以有效去除隐藏在陶瓷的晶界之间的缝隙中的微小颗粒；第三清洗过程采用超声波清洗的方式清洗陶瓷件，以去除陶瓷件上残留的颗粒和溶液(酸性或碱性溶液)，从而可以对陶瓷件进行全面清洗，最终可以有效提高清洗效果。
可以理解的是，以上实施方式仅仅是为了说明本发明的原理而采用的示例性实施方式，然而本发明并不局限于此。对于本领域内的普通技术人员而言，在不脱离本发明的精神和实质的情况下，可以做出各种变型和改进，这些变型和改进也视为本发明的保护范围。
Claims (15)
- 一种表面活性剂，用于去除陶瓷件上的颗粒，其特征在于，所述表面活性剂的组分包括：去离子水、有机磷酸类阻垢缓蚀剂、用于提高所述表面活性剂的去污力和分散性的第一有机化合物、用于去除所述陶瓷件的表面油垢的第二有机化合物、聚合磷酸盐、烷基类有机化合物以及酸性溶液。
- 根据权利要求1所述的表面活性剂，其特征在于，按重量份数计，所述去离子水为10000份；所述有机磷酸类阻垢缓蚀剂为9-11份；所述第一有机化合物为15-17份；所述第二有机化合物为9-11份；所述聚合磷酸盐为9-11份；所述烷基类有机化合物为14-16份；所述酸性溶液为9-11份。
- 根据权利要求1或2所述的表面活性剂，其特征在于，所述有机磷酸类阻垢缓蚀剂包括羟基乙叉二膦酸；所述第一有机化合物包括烷基磺酸盐；所述第二有机化合物包括乙二醇单丁醚；所述聚合磷酸盐包括琥珀酸脂磷酸盐；所述烷基类有机化合物包括烷基苯磺酸钠；所述酸性溶液包括氯化氢溶液。
- 根据权利要求3所述的表面活性剂，其特征在于，按重量份数计，所述去离子水为10000份；所述羟基乙叉二膦酸为10份；所述烷基磺酸盐为15份；所述乙二醇单丁醚为10份；所述琥珀酸脂磷酸盐为10份；所述烷基苯磺酸钠为15份；所述氯化氢溶液为10份。
- 根据权利要求3所述的表面活性剂，其特征在于，所述氯化氢溶液中氯化氢的浓度大于等于40％，且小于等于60％。
- 一种表面活性剂的制备方法，其特征在于，用于制备权利要求1-5 任意一项所述的表面活性剂；所述制备方法包括以下步骤：S1、将所述去离子水加入反应容器中；S2、按时间的先后顺序依次将所述有机磷酸类阻垢缓蚀剂、所述第一有机化合物、所述第二有机化合物、所述聚合磷酸盐、所述烷基类有机化合物以及所述酸性溶液加入所述反应容器中，并在加入每个所述组分的过程中对所述反应容器中的溶液进行搅拌。
- 根据权利要求6所述的表面活性剂的制备方法，其特征在于，所述步骤S2，还包括：在加入每个所述组分之后，且在加入下一个所述组分之前，对所述反应容器中的溶液进行搅拌。
- 根据权利要求7所述的表面活性剂的制备方法，其特征在于，在加入每个所述组分之后，且在加入下一个所述组分之前，对所述反应容器中的溶液进行搅拌的时间大于等于3min，且小于等于5min。
- 根据权利要求6所述的表面活性剂的制备方法，其特征在于，所述步骤S2中，在加入每个所述组分的过程中，使用自动的搅拌工具对所述反应容器中的溶液进行搅拌，且所述搅拌工具的转速大于等于3转/分钟，且小于等于5转/分钟。
- 根据权利要求6所述的表面活性剂的制备方法，其特征在于，在所述步骤S1中，所述去离子水的温度大于等于42℃，且小于等于50℃。
- 一种陶瓷件清洗方法，其特征在于，包括：第一清洗过程，采用化学溶液溶解陶瓷件上的颗粒；第二清洗过程，采用权利要求1-5任意一项所述的表面活性剂清洗所述 陶瓷件的整个表面，以去除微小颗粒；第三清洗过程，采用超声波清洗的方式清洗所述陶瓷件，以去除所述陶瓷件上残留的颗粒和溶液。
- 根据权利要求11所述的陶瓷件清洗方法，其特征在于，所述第一清洗过程具体包括以下步骤：S101、将陶瓷件浸泡在碱性脱脂剂中；S102、将在所述碱性脱脂剂中浸泡后的所述陶瓷件浸泡在去离子水中；S103、使用指定压力的去离子水喷淋在所述去离子水中浸泡后的所述陶瓷件的整个表面；S104、将喷淋后的所述陶瓷件浸泡在酸性溶液中；S105、将浸泡在所述酸性溶液中的所述陶瓷件浸泡在去离子水中；S106、使用所述指定压力的去离子水喷淋在所述去离子水中浸泡后的所述陶瓷件的整个表面。
- 根据权利要求11所述的陶瓷件清洗方法，其特征在于，所述第二清洗过程包括：将完成所述第一清洗过程的所述陶瓷件浸泡在所述表面活性剂中，并在所述表面活性剂中擦拭所述陶瓷件的整个表面至少3次。
- 根据权利要求11所述的陶瓷件清洗方法，其特征在于，所述第三清洗过程包括以下步骤：S301、将完成所述第二清洗过程的所述陶瓷件浸泡在去离子水中，并进行超声波清洗；S302、将超声波清洗后的所述陶瓷件浸泡在去离子水中，其中，所述步骤S302采用的去离子水的电阻率高于所述步骤S301采用的去离子水的电阻率；所述步骤S302采用的去离子水的温度高于所述步骤S301采用的去离子 水的温度；S303、对清洗后的所述陶瓷件进行吹扫，并在吹扫后对所述陶瓷件进行烘烤。
- 根据权利要求11-14任一所述的陶瓷件清洗方法，其特征在于，所述陶瓷件包括用于半导体设备的陶瓷工艺套件。
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