CN113414167B - Surfactant, preparation method thereof and ceramic part cleaning method - Google Patents
Surfactant, preparation method thereof and ceramic part cleaning method Download PDFInfo
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- CN113414167B CN113414167B CN202110699067.9A CN202110699067A CN113414167B CN 113414167 B CN113414167 B CN 113414167B CN 202110699067 A CN202110699067 A CN 202110699067A CN 113414167 B CN113414167 B CN 113414167B
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- 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
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- 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
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- 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
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- 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
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- 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
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Abstract
The embodiment of the application provides a surfactant, a preparation method thereof and a ceramic part cleaning method, wherein the surfactant is used for removing particles on a ceramic part and comprises the following components: deionized water, an organic phosphoric acid scale and corrosion inhibitor, a first organic compound for improving the detergency and the dispersibility of a surfactant, a second organic compound for removing oil scale on the surface of a ceramic part, a polymerized phosphate, an alkyl organic compound and an acidic solution. The surfactant, the preparation method thereof and the technical scheme of the ceramic part cleaning method can effectively remove particles on the ceramic part, particularly tiny particles hidden in gaps among crystal boundaries of ceramic, so that the problem that the number of ceramic particles exceeds the standard can be solved, and the chip yield is improved.
Description
Technical Field
The application relates to the technical field of semiconductor processing, in particular to a surfactant, a preparation method thereof and a ceramic part cleaning method.
Background
Contamination is a non-negligible factor in the fabrication of integrated circuits, and it is counted that 50% yield loss is derived from contamination, and particle contamination is one of the main sources of contamination. When particles adhere to the wafer surface, buried defects may be formed during film deposition, transfer of the lithographic pattern to the film pattern may be blocked during etching, and disconnection of the wires and conduction of adjacent wires may be caused in the latter part of the process. In general, if the particle size exceeds 50% of the minimum feature size of the device, there is a possibility that the device may fail. Therefore, with the continuous miniaturization requirement of integrated circuits and the increase of process difficulty, the control of particle pollution is a necessary condition for ensuring the production efficiency and the product yield.
Alumina ceramics are a ceramic made of alumina (Al 2 O 3 ) The ceramic material which is the main body is the most stable substance in oxide, has the advantages of high temperature resistance, corrosion resistance, wear resistance, high mechanical strength, high hardness, high electrical insulation property, low dielectric loss and the like, and the alumina ceramic material is increasingly applied to semiconductor equipment. However, this material inevitably generates some powdery particles on the surface during the forming process of granulation, sintering, machining, etc., and these particles once dropped on the wafer during the semiconductor manufacturing process may affect the process results, such as conduction of different wires, disconnection of the same wire, formation of voids, and the like, causing greater energy consumption and heat generation. These particles, if not removed, can severely impact process results and chip yield.
In order to remove particles on the ceramic piece, the ceramic piece needs to be cleaned, however, the existing cleaning method for the ceramic piece generally adopts an acidic solution, an alkaline solution and deionized water to clean, and as many tiny particles are hidden in gaps among grain boundaries of the ceramic piece, the acidic solution, the alkaline solution and the deionized water are difficult to enter the gaps, so that the tiny particles cannot be cleaned effectively. The detection shows that the particle number of the ceramic piece obtained by the existing ceramic piece cleaning method is more than or equal to 50ea per unit area, which falls on the wafer in the process, and is far higher than the particle index (the particle number per unit area is less than 2 ea).
Disclosure of Invention
The application aims at solving at least one of the technical problems in the prior art, and provides a surfactant, a preparation method thereof and a ceramic part cleaning method, which can effectively remove particles on a ceramic part, especially tiny particles hidden in gaps between crystal boundaries of the ceramic, so that the problem that the number of the ceramic particles exceeds the standard can be solved, and the chip yield is improved.
To achieve the above object, the present application provides a surfactant for removing particles on a ceramic member, the surfactant comprising the components of: deionized water, an organic phosphoric acid scale and corrosion inhibitor, a first organic compound for improving the detergency and the dispersibility of the surfactant, a second organic compound for removing oil scale on the surface of the ceramic part, a polyphosphate, an alkyl organic compound and an acidic solution.
Optionally, 10000 parts of deionized water are calculated according to parts by weight; 9-11 parts of organic phosphoric acid scale and corrosion inhibitor; 15-17 parts of a first organic compound; 9-11 parts of a second organic compound; 9-11 parts of polymerized phosphate; 14-16 parts of alkyl organic compound; the acid solution is 9-11 parts.
Optionally, the organic phosphoric acid scale and corrosion inhibitor comprises hydroxyethylidene diphosphonic acid; the first organic compound comprises an alkyl sulfonate; the second organic compound comprises ethylene glycol monobutyl ether;
the polymeric phosphate comprises succinate phosphate; the alkyl organic compound comprises sodium alkyl benzene sulfonate; the acidic solution comprises a hydrogen chloride solution.
Optionally, 10000 parts of deionized water are calculated according to parts by weight; 10 parts of hydroxyethylidene diphosphonic acid; 15 parts of alkyl sulfonate; 10 parts of ethylene glycol monobutyl ether;
10 parts of succinate phosphate; 15 parts of sodium alkylbenzenesulfonate; the hydrogen chloride solution is 10 parts.
Optionally, the concentration of hydrogen chloride in the hydrogen chloride solution is 40% -60%.
As another technical scheme, the embodiment of the application also provides a preparation method of the surfactant, which is used for preparing the surfactant provided by the embodiment of the application; the preparation method comprises
The method comprises the following steps:
s1, adding the deionized water into a reaction container;
s2, sequentially adding the organic phosphoric acid scale and corrosion inhibitor, the first organic compound, the second organic compound, the polyphosphate, the alkyl organic compound and the acidic solution into the reaction container according to the time sequence, and stirring the solution in the reaction container in the process of adding each component.
Optionally, the step S2 further includes:
after each of the components is added, and before the next component is added, the solution in the reaction vessel is stirred.
Optionally, after each of the components is added and before the next of the components is added, the solution in the reaction vessel is stirred for 3min or more and 5min or less.
Optionally, in step S2, during the process of adding each component, an automatic stirring tool is used to stir the solution in the reaction container, and the rotation speed of the stirring tool is 3 rpm or more and 5 rpm or less.
Optionally, in the step S1, the temperature of the deionized water is 42 ℃ or higher and 50 ℃ or lower.
As another technical solution, an embodiment of the present application further provides a method for cleaning a ceramic piece, including:
a first cleaning process, in which particles on the ceramic piece are dissolved by using a chemical solution;
a second cleaning process, in which the surfactant provided by the embodiment of the application is used for cleaning the whole surface of the ceramic piece so as to remove tiny particles;
and a third cleaning process, namely cleaning the ceramic piece in an ultrasonic cleaning mode so as to remove residual particles and solution on the ceramic piece.
Optionally, the first cleaning process specifically includes the following steps:
s101, soaking a ceramic piece in an alkaline degreasing agent;
s102, soaking the ceramic piece soaked in the alkaline degreasing agent in deionized water;
s103, spraying deionized water with specified pressure on the whole surface of the ceramic piece after being soaked in the deionized water;
s104, soaking the sprayed ceramic piece in an acidic solution;
s105, soaking the ceramic piece soaked in the acid solution in deionized water;
s106, spraying the deionized water with the specified pressure on the whole surface of the ceramic piece after being soaked in the deionized water.
Optionally, the second cleaning process includes:
immersing the ceramic member having completed the first cleaning process in the surfactant, and wiping the entire surface of the ceramic member in the surfactant at least 3 times.
Optionally, the third cleaning process includes the steps of:
s301, soaking the ceramic piece subjected to the second cleaning process in deionized water, and performing ultrasonic cleaning;
s302, soaking the ceramic piece subjected to ultrasonic cleaning in deionized water, wherein the resistivity of the deionized water adopted in the step S302 is higher than that of the deionized water adopted in the step S301; the temperature of the deionized water adopted in the step S302 is higher than that of the deionized water adopted in the step S301;
s303, purging the cleaned ceramic piece, and baking the ceramic piece after purging.
Optionally, the ceramic part comprises a ceramic process kit for a semiconductor device.
The application has the beneficial effects that:
in the technical scheme of the surfactant and the preparation method thereof provided by the embodiment of the application, the surfactant comprises the following components: deionized water, an organic phosphoric acid scale and corrosion inhibitor, a first organic compound for improving the detergency and the dispersibility of a surfactant, a second organic compound for removing oil scale on the surface of a ceramic part, a polymerized phosphate, an alkyl organic compound and an acidic solution. Surfactants containing the above components are negatively charged or anionic, so that particles on ceramic parts that are positively charged as tested in polarity can be effectively removed; in addition, the surfactant containing the components has fixed hydrophilic and lipophilic groups, can be directionally arranged on the surface of liquid (deionized water), and particularly can obviously reduce the surface tension of the liquid, so that the liquid can infiltrate into gaps among ceramic grain boundaries to clean and remove hidden particles in the gaps, thereby solving the problem that the number of ceramic particles exceeds the standard and improving the chip yield.
According to the ceramic piece cleaning method provided by the embodiment of the application, the cleaning is divided into three cleaning processes, wherein the first cleaning process adopts a chemical solution to dissolve particles on the ceramic piece, and the process can effectively clean the particles with larger size on the surface of the ceramic piece at blind holes, folds and non-welding gaps; the second cleaning process adopts the surfactant provided by the embodiment of the application to clean the whole surface of the ceramic piece, so that tiny particles hidden in gaps among grain boundaries of the ceramic can be effectively removed; and the third cleaning process adopts an ultrasonic cleaning mode to clean the ceramic part so as to remove particles and solution (acidic or alkaline solution) remained on the ceramic part, thereby comprehensively cleaning the ceramic part and finally effectively improving the cleaning effect.
Drawings
FIG. 1 is a flow chart of a method for preparing a surfactant according to a second embodiment of the present application;
FIG. 2 is a block flow diagram of a method for cleaning ceramic parts according to a third embodiment of the present application;
FIG. 3 is a flow chart of a first cleaning process according to a third embodiment of the present application;
FIG. 4 is a flow chart of a third cleaning process according to a third embodiment of the present application;
FIG. 5 is an electron microscope scan of a ceramic part obtained using a prior art ceramic part cleaning method;
fig. 6 is an electron microscope scan of a ceramic part obtained by the ceramic part cleaning method according to the embodiment of the application.
Detailed Description
In order to enable those skilled in the art to better understand the technical scheme of the application, the surfactant, the preparation method thereof and the ceramic cleaning method provided by the embodiment of the application are described in detail below with reference to the accompanying drawings.
First embodiment
The surfactant provided in this embodiment is used to remove particles from ceramic parts, including, for example, ceramic process kits for semiconductor devices. The ceramic process kit can be components made of ceramic materials such as a liner, a dielectric window, a nozzle, a screen, main and auxiliary dielectric barrels of a three-dimensional induction coil, a protective barrel of a viewing window, and the like.
The inventor conducts polarity test on the ceramic piece, and discovers that the ceramic piece is microscopically expressed as polar molecules and positively charged. The application relates to surfactants belonging to the negative or anionic group of surfactants.
Specifically, the components of the surfactant include: deionized water, an organic phosphoric acid scale and corrosion inhibitor, a first organic compound for improving the detergency and the dispersibility of a surfactant, a second organic compound for removing oil scale on the surface of a ceramic part, a polymerized phosphate, an alkyl organic compound and an acidic solution.
Wherein, the organic phosphoric acid scale and corrosion inhibitor has better cleaning effect when cleaning ceramic parts. Optionally, the organic phosphoric acid scale and corrosion inhibitor preferably comprises hydroxyethylidene diphosphonic acid, which has a larger dissociation constant (namely, polarity parameter of solute with a certain dissociation degree in aqueous solution) in deionized water, and has better cleaning effect.
The first organic compound is used to improve detergency and dispersibility of the surfactant, and it is possible to employ an organic compound having good detergency, foamability, emulsifying ability and wetting ability, for example, the first organic compound preferably includes an alkyl sulfonate, which is easily soluble in deionized water, and has good detergency and dispersibility.
The second organic compound is used for removing the surface oil dirt of the ceramic parts, and an organic compound solvent which can remove the surface oil dirt of materials such as metal, fabric, glass, plastic and the like can be used, for example, the second organic compound preferably comprises ethylene glycol monobutyl ether, which can be used as an excellent solvent and can effectively remove the dirt of non-metal surfaces (especially ceramic surfaces).
The polymeric phosphate has excellent oil solubility and can be used as a solubilizing, emulsifying and dispersing agent with excellent performance. The polymeric phosphate preferably includes succinate phosphate, which has excellent emulsifying, wetting and penetrating properties.
The alkyl-based organic compound has the functions of decontamination, wetting, foaming, emulsification, dispersion, and the like, and preferably comprises sodium alkylbenzenesulfonate.
The acidic solution is used for softening ceramic particles and neutralizing the pH of ceramics, and can be a strong acid solution which is easily volatile and soluble in water, such as hydrogen chloride solution.
Surfactants containing the above components are negatively charged or anionic, so that particles on ceramic parts that are positively charged as tested in polarity can be effectively removed; in addition, the surfactant containing the components has fixed hydrophilic and lipophilic groups, can be directionally arranged on the surface of liquid (namely deionized water), and particularly can obviously reduce the surface tension of the liquid, so that the liquid can infiltrate into gaps between ceramic grain boundaries to clean and remove hidden particles in the gaps, thereby solving the problem that the number of ceramic particles exceeds the standard and improving the chip yield.
In some preferred embodiments, optionally, the deionized water is 10000 parts by weight; 9-11 parts of organic phosphoric acid scale and corrosion inhibitor; 15-17 parts of a first organic compound; 9-11 parts of a second organic compound; 9-11 parts of polymerized phosphate; 14-16 parts of alkyl organic compounds; the acid solution is 9-11 parts.
In some preferred embodiments, the components of the surfactant described above optionally include: deionized water, hydroxyethylidene diphosphonic acid, alkyl sulfonate, ethylene glycol monobutyl ether, succinate phosphate, sodium alkylbenzenesulfonate, and hydrogen chloride solution. The surfactant comprising the above components is more effective in removing particles from ceramic parts that are positively charged when tested for polarity.
In some preferred embodiments, optionally, the deionized water is 10000 parts by weight; 10 parts of hydroxyethylidene diphosphonic acid; 15 parts of alkyl sulfonate; ethylene glycol monobutyl ether 10 parts; 10 parts of succinate phosphate; 15 parts of sodium alkylbenzenesulfonate; the hydrogen chloride solution was 10 parts.
In some preferred embodiments, the concentration of hydrogen chloride in the hydrogen chloride solution is optionally 40% -60%, preferably 50%. The concentration of hydrogen chloride is simply referred to as the concentration of hydrogen chloride in the amount.
Second embodiment
The preparation method of the surfactant provided by the embodiment is used for preparing the surfactant provided by the embodiment. As shown in fig. 1, the preparation method comprises the following steps:
s1, adding deionized water into a reaction container;
optionally, in the step S1, the temperature of the deionized water is 42 ℃ or higher and 50 ℃ or lower. By setting the temperature of deionized water within this range, a temperature atmosphere that facilitates rapid dissolution of the added components can be created.
S2, sequentially adding the organic phosphoric acid scale and corrosion inhibitor, the first organic compound, the second organic compound, the polyphosphate, the alkyl organic compound and the acidic solution into the reaction container according to the time sequence, and stirring the solution in the reaction container in the process of adding each component.
In some preferred embodiments, optionally, in step S2 above, the hydroxyethylidene bisphosphonic acid, the alkyl sulfonate, the ethylene glycol monobutyl ether, the succinate phosphate, the sodium alkylbenzenesulfonate, and the hydrogen chloride solution are added to the reaction vessel in chronological order, and the solution in the reaction vessel is stirred during the addition of each component.
Specifically, during each addition of one of the components, the solution in the reaction vessel is continuously stirred to accelerate the dissolution of the component. In practice, the solution in the reaction vessel may be stirred using an automatic or manual stirring tool.
In some preferred embodiments, optionally, in the step S2, the solution in the reaction vessel is stirred using an automatic stirring tool during the addition of each component, and the rotation speed of the stirring tool is 3 rpm or more and 5 rpm or less. In this way, dissolution of the components can be effectively accelerated.
In some preferred embodiments, optionally, step S2 above further includes:
after each component was added, the solution in the reaction vessel was stirred.
That is, not only is the solution in the reaction vessel stirred during the addition of each component, but also the solution in the reaction vessel is stirred after the addition of each component and before the addition of the next component, which can further enhance the dissolution effect of the components.
Optionally, the solution in the reaction vessel is stirred for 3min or more and 5min or less after each component is added and before the next component is added.
The surfactant provided in this example can be obtained after the last component is added to the reaction vessel and the corresponding stirring is completed.
The preparation method of the surfactant provided by the embodiment is safe, efficient, simple in process and easy to realize.
Third embodiment
Referring to fig. 2, the present embodiment provides a method for cleaning a ceramic part, which includes:
a first cleaning process, in which particles on the ceramic piece are dissolved by using a chemical solution;
the first cleaning process can effectively clean particles on the surface of the ceramic part, in particular to clean particles on blind holes, folds and non-welding gaps with larger sizes on the surface of the ceramic part.
A second cleaning process of cleaning the entire surface of the ceramic member with the surfactant provided in this embodiment to remove minute particles;
the surfactant provided by the embodiment is negatively charged or anionic, and the polar molecules of the ceramic piece are positively charged, so that the surfactant can effectively remove particles on the ceramic piece; in addition, the surfactant provided by the embodiment has fixed hydrophilic and lipophilic groups, can be arranged on the surface of the liquid in an oriented manner, and particularly can enable the surface tension of the liquid to be obviously reduced, so that the liquid can infiltrate into gaps between ceramic grain boundaries, and particles hidden in the gaps can be cleaned and removed, and the number of the particles can be greatly reduced.
And a third cleaning process, namely cleaning the ceramic piece in an ultrasonic cleaning mode to remove residual particles and solution on the ceramic piece.
Ultrasonic cleaning refers to cleaning of particles on a ceramic material by water waves generated by ultrasonic vibration. The ceramic part can be comprehensively cleaned in the third cleaning process, and finally the cleaning effect can be effectively improved.
A detailed description of the first cleaning process is provided below. Specifically, as shown in fig. 3, the first cleaning process specifically includes the following steps:
s101, soaking a ceramic piece in an alkaline degreasing agent;
the alkaline degreasing agent may dissolve particles on the ceramic part.
In order to effectively dissolve the particles on the ceramic part and improve the cleaning effect, optionally, in the step S101, the time for immersing the ceramic part in the alkaline degreasing agent is in a range of 50min or more and 80min or less.
S102, soaking the ceramic piece soaked in the alkaline degreasing agent in deionized water;
the step S102 is used for cleaning the alkaline degreasing agent on the ceramic part, so as to avoid damage to the sealing surface and the hole edge of the ceramic part caused by the alkaline degreasing agent and influence on the tightness of the part.
S103, spraying deionized water with specified pressure on the whole surface of the ceramic piece soaked in the deionized water;
the step S103 is used to further remove particles and residual solution on the ceramic member.
In order to further improve the cleaning effect, the above specified pressure may be in the range of 40psi or more and 60psi or less.
S104, soaking the sprayed ceramic piece in an acid solution;
the step S104 can neutralize the alkaline solution remained on the ceramic piece to reduce the corrosion of the alkaline solution to the ceramic piece and avoid the damage of the alkaline solution to the sealing surface and the hole edge of the ceramic piece.
Optionally, in step S104, the time period for immersing the ceramic part in the acidic solution is in a range of 5min or more and 10min or less.
Optionally, the acidic solution is hydrochloric acid or a fluoronitric acid solution, wherein the fluoronitric acid solution has better dissolution with an alkaline solution (such as KOH solution).
S105, soaking the ceramic piece soaked in the acid solution in deionized water;
the step S105 is used to clean the acidic solution on the ceramic part.
S106, spraying the deionized water with the specified pressure on the whole surface of the ceramic piece soaked in the deionized water.
The step S106 is used to further remove particles and residual solution on the ceramic member.
In order to further improve the cleaning effect, the above specified pressure may be in the range of 40psi or more and 60psi or less.
Optionally, the second cleaning process includes:
immersing the ceramic member having completed the first cleaning process in the surfactant, and wiping the entire surface of the ceramic member at least 3 times in the surfactant.
That is, the ceramic member is always immersed in the surfactant during wiping of the entire surface of the ceramic member, which is more advantageous in that liquid is infiltrated into gaps between the grain boundaries of the ceramic member to wash out particles hidden in the gaps.
The ceramic piece is soaked in the surfactant, and the ceramic piece is wiped until the whole surface is wiped, wherein the process is 1 st time; the ceramic part is then re-immersed in the unused surfactant and wiped until the entire surface is wiped, the process being 2 nd time, and so on.
A detailed description of the third cleaning process is provided below. Specifically, as shown in fig. 4, the third cleaning process specifically includes the steps of:
s301, soaking the ceramic piece subjected to the second cleaning process in deionized water, and performing ultrasonic cleaning;
optionally, in step S301, the range of resistivity of the deionized water is equal to or greater than 2mΩ·cm, and the range of cleaning time is equal to or greater than 10min, and equal to or less than 15min.
The step S301 can clean the ceramic part comprehensively, and the cleaning effect of the ceramic part can be ensured to meet the process requirement after the ultrasonic cleaning step is completed because the cleaning effect of ultrasonic cleaning by using deionized water is most obvious. Furthermore, the removal of the particles on the surface of the ceramic member and the minute particles in the gaps between the ceramic grain boundaries has been achieved by the foregoing first cleaning process and second cleaning process, so that the particles which cannot be removed can be removed before the ultrasonic cleaning is performed.
S302, soaking the ceramic piece subjected to ultrasonic cleaning in deionized water;
wherein the resistivity of deionized water used in the step S302 is higher than that of deionized water used in the step S301, for example, the resistivity of deionized water in the step S301 is in a range of 2mΩ·cm or more, and the resistivity of deionized water in the step S302 is in a range of 4mΩ·cm or more.
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. For example, the temperature of the deionized water used in the step S302 is normal temperature (typically 25 ℃) and the temperature of the deionized water used in the step S301 is in the range of 32 ℃ or higher and 42 ℃ or lower.
In order to improve the cleaning effect, optionally, new deionized water is always introduced into the cleaning tank in the soaking process, and the deionized water in the cleaning tank is discharged in an overflow mode, so that the deionized water is in a circulating flow state, and the cleaning effect can be further improved.
S303, purging the soaked ceramic piece, and baking the ceramic piece after purging.
Optionally, the purge gas used in the step S303 includes nitrogen, and the purity of the nitrogen is 99.999%; the included angle between the nitrogen purging direction and the surface of the ceramic part is, for example, 30 degrees or more and 45 degrees or less, so as to avoid particles from falling on the surface of the ceramic part again.
Optionally, the ceramic part is first thoroughly purged with dry nitrogen; the clean-up oven (or oven) is then purged with dry nitrogen to dry the interior thereof; and finally, placing the ceramic piece into a purged purifying furnace (or oven) for baking.
The following is a comparative experiment performed on ceramic pieces obtained by the ceramic piece cleaning method in the prior art and the ceramic piece cleaning method provided by the embodiment of the present application. Specifically, the ceramic part cleaning method in the prior art comprises the following steps: firstly, immersing a ceramic part in an alkaline degreasing agent for 50-80 min, and then placing the ceramic part in deionized water for rinsing (pressurized deionized water is used for spraying all the positions on the surface of the ceramic part); then, immersing the ceramic piece in an acidic solution for 5-10 min, taking out the ceramic piece from the solution, immersing the ceramic piece in deionized water again for the rinsing, immersing the ceramic piece in deionized water with resistivity greater than or equal to 4MΩ & cm and normal temperature for ultrasonic cleaning for 10-15 min, immersing the ceramic piece in deionized water with resistivity greater than or equal to 8MΩ & cm for hot water immersion cleaning, finally drying the ceramic piece by using nitrogen, and drying the ceramic piece to complete the whole cleaning process.
The ceramic piece cleaning method provided by the embodiment of the application comprises the three cleaning processes, wherein the first cleaning process comprises the steps S101-S106; the second cleaning process comprises the steps of immersing the sprayed ceramic piece in the surfactant, and wiping the whole surface of the ceramic piece at least 3 times in the surfactant; the third cleaning process includes the above steps S301 to S303.
Fig. 5 is an electron microscope scan of a ceramic part obtained by a prior art ceramic part cleaning method. Fig. 6 is an electron microscope scan of a ceramic part obtained by the ceramic part cleaning method according to the embodiment of the application. As can be seen from comparing fig. 5 and fig. 6, the surface of the ceramic piece obtained by the ceramic piece cleaning method in the prior art still has suspended particles, as shown in fig. 5 (a) and (b), wherein white dots on the black area are suspended particles. In addition, the ceramic piece obtained by the ceramic piece cleaning method in the prior art has the particle number of particles falling on a wafer per unit area more than or equal to 50ea in the process and is far higher than the particle index (the particle number of particles per unit area is less than 2 ea). In contrast, as can be seen from fig. 6 (a) and (b), white dots on the black area in the graph are significantly reduced, so that it can be seen that suspended particles on a ceramic piece obtained by the ceramic piece cleaning method provided by the embodiment of the present application are significantly reduced, and the number of particles per unit area of the ceramic piece falling on a wafer during the process is lower than the particle index (the number of particles per unit area is <2 ea).
The ceramic part in this embodiment includes, for example, a ceramic process kit for a semiconductor device. The ceramic process kit can be components made of ceramic materials such as a liner, a dielectric window, a nozzle, a screen, main and auxiliary dielectric barrels of a three-dimensional induction coil, a protective barrel of a viewing window, and the like.
In summary, the method for cleaning a ceramic part provided in this embodiment divides cleaning into three cleaning processes, wherein the first cleaning process adopts a chemical solution to dissolve particles on the ceramic part, and the process can effectively clean particles with larger size at blind holes, folds and non-welding gaps on the surface of the ceramic part; the second cleaning process adopts the surfactant provided by the embodiment to clean the whole surface of the ceramic piece, so that tiny particles hidden in gaps among grain boundaries of the ceramic can be effectively removed; and the third cleaning process adopts an ultrasonic cleaning mode to clean the ceramic part so as to remove particles and solution (acidic or alkaline solution) remained on the ceramic part, thereby comprehensively cleaning the ceramic part and finally effectively improving the cleaning effect.
It is to be understood that the above embodiments are merely illustrative of the application of the principles of the present application, but not in limitation thereof. Various modifications and improvements may be made by those skilled in the art without departing from the spirit and substance of the application, and are also considered to be within the scope of the application.
Claims (18)
1. A surfactant for removing particles from a ceramic article, the surfactant comprising: deionized water, an organic phosphoric acid scale and corrosion inhibitor, a first organic compound for improving the detergency and the dispersibility of the surfactant, a second organic compound for removing oil scale on the surface of the ceramic part, a polyphosphate, an alkyl organic compound and an acidic solution;
the organic phosphoric acid scale and corrosion inhibitor comprises hydroxyethylidene diphosphonic acid; the first organic compound comprises an alkyl sulfonate; the second organic compound comprises ethylene glycol monobutyl ether; the polymeric phosphate comprises succinate phosphate; the alkyl organic compound comprises sodium alkyl benzene sulfonate; the acidic solution comprises a hydrogen chloride solution.
2. The surfactant according to claim 1, wherein the deionized water is 10000 parts by weight; 9-11 parts of organic phosphoric acid scale and corrosion inhibitor; 15-17 parts of a first organic compound; 9-11 parts of a second organic compound; 9-11 parts of polymerized phosphate; 14-16 parts of alkyl organic compound; the acid solution is 9-11 parts.
3. The surfactant according to claim 1, wherein the deionized water is 10000 parts by weight; 10 parts of hydroxyethylidene diphosphonic acid; 15 parts of alkyl sulfonate; 10 parts of ethylene glycol monobutyl ether; 10 parts of succinate phosphate; 15 parts of sodium alkylbenzenesulfonate; the hydrogen chloride solution is 10 parts.
4. The surfactant of claim 1, wherein the concentration of hydrogen chloride in the hydrogen chloride solution is 40% -60%.
5. A process for preparing a surfactant according to any one of claims 1 to 4; the preparation method comprises the following steps:
s1, adding the deionized water into a reaction container;
s2, sequentially adding the organic phosphoric acid scale and corrosion inhibitor, the first organic compound, the second organic compound, the polyphosphate, the alkyl organic compound and the acidic solution into the reaction container according to the time sequence, and stirring the solution in the reaction container in the process of adding each component.
6. The method for preparing a surfactant according to claim 5, wherein the step S2 further comprises:
after each of the components is added, and before the next component is added, the solution in the reaction vessel is stirred.
7. The method for producing a surfactant according to claim 6, wherein the solution in the reaction vessel is stirred for 3min or more and 5min or less after each of the components is added and before the next of the components is added.
8. The method according to claim 5, wherein in the step S2, the solution in the reaction vessel is stirred by using an automatic stirring tool during the addition of each of the components, and the rotation speed of the stirring tool is 3 rpm or more and 5 rpm or less.
9. The method according to claim 5, wherein in the step S1, the deionized water is at a temperature of 42 ℃ or higher and 50 ℃ or lower.
10. A method for cleaning ceramic parts, comprising:
a first cleaning process, in which particles on the ceramic piece are dissolved by using a chemical solution;
a second cleaning process of cleaning the entire surface of the ceramic member with a surfactant to remove minute particles; the components of the surfactant comprise: deionized water, an organic phosphoric acid scale and corrosion inhibitor, a first organic compound for improving the detergency and the dispersibility of the surfactant, a second organic compound for removing oil scale on the surface of the ceramic part, a polyphosphate, an alkyl organic compound and an acidic solution;
and a third cleaning process, namely cleaning the ceramic piece in an ultrasonic cleaning mode to remove residual particles and solution on the ceramic piece, so that the number of particles per unit area of the ceramic piece falling on a wafer in the process is lower than 2ea.
11. The method for cleaning ceramic parts according to claim 10, wherein the deionized water is 10000 parts by weight; 9-11 parts of organic phosphoric acid scale and corrosion inhibitor; 15-17 parts of a first organic compound; 9-11 parts of a second organic compound; 9-11 parts of polymerized phosphate; 14-16 parts of alkyl organic compound; the acid solution is 9-11 parts.
12. The method for cleaning ceramic parts according to claim 10, wherein the organic phosphoric acid scale and corrosion inhibitor comprises hydroxyethylidene diphosphonic acid; the first organic compound comprises an alkyl sulfonate; the second organic compound comprises ethylene glycol monobutyl ether; the polymeric phosphate comprises succinate phosphate; the alkyl organic compound comprises sodium alkyl benzene sulfonate; the acidic solution comprises a hydrogen chloride solution.
13. The method for cleaning ceramic parts according to claim 12, wherein the deionized water is 10000 parts by weight; 10 parts of hydroxyethylidene diphosphonic acid; 15 parts of alkyl sulfonate; 10 parts of ethylene glycol monobutyl ether; 10 parts of succinate phosphate; 15 parts of sodium alkylbenzenesulfonate; the hydrogen chloride solution is 10 parts.
14. The method of claim 12, wherein the concentration of hydrogen chloride in the hydrogen chloride solution is 40% -60%.
15. The method for cleaning ceramic parts according to any one of claims 10 to 14, wherein the first cleaning process comprises the steps of:
s101, soaking a ceramic piece in an alkaline degreasing agent;
s102, soaking the ceramic piece soaked in the alkaline degreasing agent in deionized water;
s103, spraying deionized water with specified pressure on the whole surface of the ceramic piece after being soaked in the deionized water;
s104, soaking the sprayed ceramic piece in an acidic solution;
s105, soaking the ceramic piece soaked in the acid solution in deionized water;
s106, spraying the deionized water with the specified pressure on the whole surface of the ceramic piece after being soaked in the deionized water.
16. The method of any one of claims 10-14, wherein the second cleaning process comprises:
immersing the ceramic member having completed the first cleaning process in the surfactant, and wiping the entire surface of the ceramic member in the surfactant at least 3 times.
17. The method of cleaning ceramic ware according to any one of claims 10-14, wherein the third cleaning process comprises the steps of:
s301, soaking the ceramic piece subjected to the second cleaning process in deionized water, and performing ultrasonic cleaning;
s302, soaking the ceramic piece subjected to ultrasonic cleaning in deionized water, wherein the resistivity of the deionized water adopted in the step S302 is higher than that of the deionized water adopted in the step S301; the temperature of the deionized water adopted in the step S302 is higher than that of the deionized water adopted in the step S301;
s303, purging the cleaned ceramic piece, and baking the ceramic piece after purging.
18. The method of any one of claims 10-14, wherein the ceramic part comprises a ceramic process kit for a semiconductor device.
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| CN202110699067.9A CN113414167B (en) | 2021-06-23 | 2021-06-23 | Surfactant, preparation method thereof and ceramic part cleaning method |
| TW111121832A TWI813333B (en) | 2021-06-23 | 2022-06-13 | Surfactant, preparation method thereof and cleaning method of ceramic parts |
| PCT/CN2022/098381 WO2022267916A1 (en) | 2021-06-23 | 2022-06-13 | Surfactant, preparation method therefor, and method for cleaning ceramic part |
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| CN202110699067.9A CN113414167B (en) | 2021-06-23 | 2021-06-23 | Surfactant, preparation method thereof and ceramic part cleaning method |
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Also Published As
| Publication number | Publication date |
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| WO2022267916A1 (en) | 2022-12-29 |
| TWI813333B (en) | 2023-08-21 |
| CN113414167A (en) | 2021-09-21 |
| TW202300636A (en) | 2023-01-01 |
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