CN113414167A - 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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- CN113414167A CN113414167A CN202110699067.9A CN202110699067A CN113414167A CN 113414167 A CN113414167 A CN 113414167A CN 202110699067 A CN202110699067 A CN 202110699067A CN 113414167 A CN113414167 A CN 113414167A
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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
Abstract
The embodiment of the invention 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, organic phosphoric acid scale and corrosion inhibitors, a first organic compound for improving the detergency and the dispersibility of a surfactant, a second organic compound for removing oil dirt on the surface of a ceramic part, a polymeric phosphate, an alkyl organic compound and an acidic solution. The technical scheme of the surfactant, the preparation method thereof and the ceramic part cleaning method provided by the embodiment of the invention can effectively remove particles on the ceramic part, especially tiny particles hidden in gaps among crystal boundaries of the ceramic, thereby solving the problem that the number of the ceramic particles exceeds the standard and improving the yield of chips.
Description
Technical Field
The invention relates to the technical field of semiconductor processing, in particular to a surfactant, a preparation method thereof and a ceramic piece cleaning method.
Background
Contamination is a non-negligible factor in the fabrication of integrated circuits, and statistically, 50% of yield loss is attributed to contamination, and particle contamination is one of the major sources of contamination. The particles may become buried defects during deposition of the film layer when they are attached to the wafer surface, may block the transfer of the photo-etching pattern to the film layer pattern during etching, and may cause disconnection of the conductive lines and conduction of adjacent wires in the latter part of the process. Generally, particle sizes in excess of 50% of the minimum feature size of the device can lead to device failure. Therefore, as the demand for miniaturization of integrated circuits continues and the process difficulty increases, particle contamination control is a necessary condition for ensuring production efficiency and product yield.
The alumina ceramic is prepared from alumina (Al)2O3) The ceramic material as the main body is the most stable substance in oxide, and has the advantages of high temperature resistance, corrosion resistance, wear resistance, high mechanical strength, high hardness, high electrical insulation, low dielectric loss and the like, so that the alumina ceramic material is increasingly applied to semiconductor equipment. However, such materials inevitably produce some powdery particles on the surface during the molding 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, causing greater energy consumption and heat generation, etc. These particles, if not removed, can severely affect process results and chip yield.
However, the existing ceramic piece cleaning method generally adopts acidic solution, alkaline solution and deionized water for cleaning, and because many tiny particles are hidden in gaps among crystal boundaries of the ceramic piece, and the acidic solution, the alkaline solution and the deionized water are difficult to enter the gaps, the tiny particles cannot be effectively cleaned. The detection shows that the number of particles per unit area of the ceramic piece obtained by the existing ceramic piece cleaning method is more than or equal to 50ea and is far higher than the particle index (the number of particles per unit area is less than 2ea) in the process.
Disclosure of Invention
The invention aims to at least solve 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 among crystal boundaries of the ceramic, thereby solving the problem that the number of the ceramic particles exceeds the standard and improving the yield of chips.
In order to achieve the above object, the present invention provides a surfactant for removing particles from a ceramic article, the surfactant comprising: deionized water, organic phosphoric acid scale and corrosion inhibitors, a first organic compound for improving the detergency and the dispersibility of the surfactant, a second organic compound for removing oil dirt on the surface of the ceramic part, polymerized phosphate, alkyl organic compounds and an acidic solution.
Optionally, the deionized water is 10000 parts by weight; 9-11 parts of an organic phosphoric acid scale and corrosion inhibitor; 15-17 parts of the first organic compound; 9-11 parts of a second organic compound; 9-11 parts of polymerized phosphate; 14-16 parts of alkyl organic compound; and 9-11 parts of the acidic solution.
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 a succinate phosphate; the alkyl organic compound comprises sodium alkyl benzene sulfonate; the acidic solution comprises a hydrogen chloride solution.
Optionally, 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 alkyl benzene sulfonate; the hydrogen chloride solution is 10 parts.
Optionally, the concentration of hydrogen chloride in the hydrogen chloride solution is 40% -60%.
As another technical solution, an embodiment of the present invention further provides a method for preparing a surfactant, which is used for preparing the surfactant provided in the embodiment of the present invention; 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 polymeric phosphate, the alkyl organic compound and the acidic solution into the reaction vessel in time sequence, and stirring the solution in the reaction vessel 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 adding each of the components and before adding the next component, stirring the solution in the reaction vessel for a time period of 3min or more and 5min or less.
Optionally, in step S2, during the process of adding each of the components, an automatic stirring tool is used to stir the solution in the reaction container, and the rotation speed of the stirring tool is greater than or equal to 3 rpm and less than or equal to 5 rpm.
Optionally, in the step S1, the temperature of the deionized water is greater than or equal to 42 ℃ and less than or equal to 50 ℃.
As another technical solution, an embodiment of the present invention further provides a method for cleaning a ceramic part, including:
a first cleaning process, wherein particles on the ceramic piece are dissolved by adopting a chemical solution;
a second cleaning process, wherein the surfactant provided by the embodiment of the invention is used for cleaning the whole surface of the ceramic part so as to remove micro particles;
and in the third cleaning process, the ceramic piece is cleaned in an ultrasonic cleaning mode to remove residual particles and solution on the ceramic piece.
Optionally, the first cleaning process specifically includes the following steps:
s101, soaking the 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 soaked in the deionized water;
s104, soaking the sprayed ceramic piece in an acid solution;
s105, soaking the ceramic piece soaked in the acidic solution in deionized water;
and S106, spraying the deionized water with the specified pressure on the whole surface of the ceramic piece soaked in the deionized water.
Optionally, the second cleaning process includes:
immersing the ceramic piece having completed the first cleaning process in the surfactant, and wiping the entire surface of the ceramic piece in the surfactant at least 3 times.
Optionally, the third cleaning process includes the following steps:
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, sweeping the cleaned ceramic piece, and baking the ceramic piece after sweeping.
Optionally, the ceramic piece comprises a ceramic process kit for a semiconductor device.
The invention has the beneficial effects that:
in the technical scheme of the surfactant and the preparation method thereof provided by the embodiment of the invention, the components of the surfactant comprise: deionized water, organic phosphoric acid scale and corrosion inhibitors, a first organic compound for improving the detergency and the dispersibility of a surfactant, a second organic compound for removing oil dirt on the surface of a ceramic part, a polymeric phosphate, an alkyl organic compound and an acidic solution. The surfactant containing the above components is negatively charged or anionic, so that particles on the ceramic piece, the polarity of which is tested to be positively charged, can be effectively removed; the surfactant containing the components has fixed hydrophilic and oleophilic groups, can be directionally arranged on the surface of liquid (deionized water), and particularly can remarkably reduce the surface tension of the liquid, so that the liquid can be soaked into gaps among ceramic grain boundaries to clean and remove particles hidden in the gaps, the problem that the number of ceramic particles exceeds the standard can be solved, and the yield of chips is improved.
According to the ceramic part cleaning method provided by the embodiment of the invention, cleaning is divided into three cleaning processes, wherein a first cleaning process adopts a chemical solution to dissolve particles on the ceramic part, and the process can effectively clean particles on blind holes, folds and non-welding seams with larger sizes on the surface of the ceramic part; in the second cleaning process, the whole surface of the ceramic part is cleaned by adopting the surfactant provided by the embodiment of the invention, so that tiny particles hidden in gaps among crystal boundaries of the ceramic can be effectively removed; the third cleaning process adopts an ultrasonic cleaning mode to clean the ceramic piece so as to remove residual particles and solution (acid or alkaline solution) on the ceramic piece, so that the ceramic piece can be comprehensively cleaned, and finally, the cleaning effect can be effectively improved.
Drawings
FIG. 1 is a block flow diagram of a process for preparing a surfactant according to a second embodiment of the present invention;
FIG. 2 is a block flow diagram of a ceramic part cleaning method according to a third embodiment of the present invention;
FIG. 3 is a block flow diagram of a first cleaning process employed in a third embodiment of the present invention;
FIG. 4 is a block flow diagram of a third cleaning process employed in a third embodiment of the present invention;
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 scanning image of the ceramic part obtained by the ceramic part cleaning method according to the embodiment of the present invention.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the following describes the surfactant, the preparation method thereof, and the ceramic cleaning method provided by the embodiments of the present invention in detail with reference to the accompanying drawings.
First embodiment
The present embodiment provides a surfactant for removing particles from a ceramic article, such as a ceramic process kit for use in semiconductor devices. The ceramic process kit can be parts such as a lining, a medium window, a nozzle, a sieve tube, a main medium cylinder and an auxiliary medium cylinder of a three-dimensional induction coil, an observation window protection cylinder and the like which are made of ceramic materials.
The inventor of the application carries out polarity test on the ceramic piece, and finds that the ceramic piece is microscopically represented by polar molecules and is positively charged. The invention relates to a surfactant which belongs to a negative electricity or anion surfactant.
Specifically, the components of the above surfactant include: deionized water, organic phosphoric acid scale and corrosion inhibitors, a first organic compound for improving the detergency and the dispersibility of a surfactant, a second organic compound for removing oil dirt on the surface of a ceramic part, a polymeric phosphate, an alkyl organic compound and an acidic solution.
Wherein, the organic phosphoric acid scale and corrosion inhibitor has better cleaning effect when cleaning the ceramic parts. Optionally, the organic phosphoric acid scale and corrosion inhibitor preferably comprises hydroxyethylidene diphosphonic acid, which has a larger dissociation constant (i.e. a polarity parameter of a solute with a certain dissociation degree in an 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 may be an organic compound having better detergency, foamability, emulsifying power and wetting power, 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 oil stains on the surface of the ceramic piece, and an organic compound solvent which can remove the oil stains on the surface of metal, fabric, glass, plastic and other materials can be adopted, for example, the second organic compound preferably comprises ethylene glycol monobutyl ether, and the second organic compound can be used as an excellent solvent and can effectively remove stains on a non-metal surface (especially a ceramic surface).
The polymerized phosphate has excellent oil solubility and can be used as a solubilizing, emulsifying and dispersing agent with excellent performance. The polymeric phosphate preferably comprises a succinate phosphate which has excellent emulsifying, wetting and penetrating properties.
The alkyl organic compound preferably includes sodium alkyl benzene sulfonate, and has the effects of removing dirt, moistening, foaming, emulsifying, dispersing, and other surface activities.
The acidic solution is used for softening ceramic particles and neutralizing the pH value of the ceramic, and the acidic solution can be a volatile strong acid solution which is easily dissolved in water, such as a hydrogen chloride solution.
The surfactant containing the above components is negatively charged or anionic, so that particles on the ceramic piece, the polarity of which is tested to be positively charged, can be effectively removed; in addition, the surfactant containing the components has fixed hydrophilic and oleophilic groups, can be directionally arranged on the surface of liquid (namely deionized water), and particularly can remarkably reduce the surface tension of the liquid, so that the liquid can be soaked into gaps among ceramic grain boundaries to clean and remove particles hidden in the gaps, the problem that the number of ceramic particles exceeds the standard can be solved, and the yield of chips is improved.
In some preferred embodiments, 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; 9-11 parts of an acidic solution.
In some preferred embodiments, optionally, the surfactant comprises: deionized water, hydroxyethylidene diphosphonic acid, alkyl sulfonate, ethylene glycol monobutyl ether, succinate phosphate, sodium alkyl benzene sulfonate and hydrogen chloride solution. The surfactant comprising the above composition is more effective in removing particles on ceramic articles 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; 10 parts of ethylene glycol monobutyl ether; 10 parts of succinate phosphate; 15 parts of sodium alkyl benzene sulfonate; the hydrogen chloride solution is 10 parts.
In some preferred embodiments, the concentration of the hydrogen chloride in the hydrogen chloride solution is optionally 40% to 60%, preferably 50%. The concentration of hydrogen chloride is simply referred to as the amount concentration of hydrogen chloride.
Second embodiment
The preparation method of the surfactant provided in this example is used to prepare the surfactant provided in this example. As shown in fig. 1, the preparation method comprises the following steps:
s1, adding deionized water into the reaction container;
optionally, in step S1, the temperature of the deionized water is 42 ℃ or higher and 50 ℃ or lower. By setting the temperature of the deionized water within this range, a temperature atmosphere favorable for rapid dissolution of the added component can be created.
S2, sequentially adding the organic phosphoric acid scale and corrosion inhibitor, the first organic compound, the second organic compound, the polymeric phosphate, the alkyl organic compound and the acidic solution into the reaction vessel in time sequence, and stirring the solution in the reaction vessel in the process of adding each component.
In some preferred embodiments, optionally, in step S2, the hydroxyethylidene diphosphonic acid, the alkyl sulfonate, the ethylene glycol monobutyl ether, the succinate phosphate, the sodium alkyl benzene sulfonate and the hydrogen chloride solution are sequentially added to the reaction vessel in chronological order, and the solution in the reaction vessel is stirred during the addition of each component.
Specifically, the solution in the reaction vessel is continuously stirred during each addition of one component 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 step S2, during the process of adding each component, the solution in the reaction vessel is stirred by using an automatic stirring tool, and the rotation speed of the stirring tool is greater than or equal to 3 rpm and less than or equal to 5 rpm. In this way, the dissolution of the components can be effectively accelerated.
In some preferred embodiments, optionally, the step S2 further includes:
after each component was added, the solution in the reaction vessel was stirred.
That is, not only the solution in the reaction vessel is 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, so that the dissolving effect of the components can be further improved.
Optionally, after each component is added, and before the next component is added, the solution in the reaction vessel is stirred for a time of 3min or more and 5min or less.
The surfactant provided in this example was obtained after the last component was added to the reaction vessel and the corresponding stirring was completed.
The preparation method of the surfactant provided by the embodiment is safe, efficient, simple in process and easy to implement.
Third embodiment
Referring to fig. 2, the present embodiment provides a method for cleaning a ceramic part, which includes:
a first cleaning process, wherein particles on the ceramic piece are dissolved by adopting a chemical solution;
the first cleaning process can effectively clean particles on the surface of the ceramic part, and particularly clean particles on blind holes, folds and non-welding gaps with large sizes on the surface of the ceramic part.
A second cleaning process, in which the surfactant provided in this embodiment is used to clean the entire surface of the ceramic part to remove the fine particles;
because the surfactant provided by the embodiment is negatively charged or anionic, and the polar molecules of the ceramic part are positively charged, the surfactant can effectively remove particles on the ceramic part; in addition, the surfactant provided by the embodiment has fixed hydrophilic and oleophilic groups, can be directionally arranged on the surface of the liquid, and particularly can remarkably reduce the surface tension of the liquid, so that the liquid can infiltrate into gaps among ceramic grain boundaries to clean and remove particles hidden in the gaps, and further the number of the particles can be greatly reduced.
And in the third cleaning process, the ceramic piece is cleaned in an ultrasonic cleaning mode to remove residual particles and solution on the ceramic piece.
The ultrasonic cleaning is to clean particles on the ceramic member by water waves generated by ultrasonic oscillation. The third cleaning process can comprehensively clean the ceramic parts, and finally, the cleaning effect can be effectively improved.
A detailed description will be given below of a specific embodiment of the above-described first cleaning process. Specifically, as shown in fig. 3, the first cleaning process specifically includes the following steps:
s101, soaking the ceramic piece in an alkaline degreasing agent;
the alkaline degreasing agent can dissolve particles on the ceramic piece.
In order to effectively dissolve the particles on the ceramic member and improve the cleaning effect, optionally, in step S101, the ceramic member is soaked in the alkaline degreasing agent for a time period greater than or equal to 50min and less than or equal to 80 min.
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, and avoids 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.
S103, spraying deionized water with specified pressure on the whole surface of the ceramic piece soaked in the deionized water;
the step S103 is to further remove particles and residual solution on the ceramic piece.
In order to further improve the cleaning effect, the specified pressure is optionally in a 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 remaining on the ceramic part to reduce corrosion of the alkaline solution to the ceramic part and prevent the alkaline solution from damaging the sealing surface and the hole edge of the ceramic part.
Optionally, in step S104, the time range of the ceramic piece being soaked in the acidic solution is greater than or equal to 5min and less than or equal to 10 min.
Optionally, the acidic solution is hydrochloric acid or a fluoronitric acid solution, wherein the fluoronitric acid solution has a better dissolving effect with an alkaline solution (for example, KOH solution).
S105, soaking the ceramic piece soaked in the acidic solution in deionized water;
the step S105 is to clean the acidic solution on the ceramic piece.
And 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 piece.
In order to further improve the cleaning effect, the specified pressure is optionally in a range of 40psi or more and 60psi or less.
Optionally, the second cleaning process includes:
the ceramic piece having completed 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.
That is, during the process of wiping the whole surface of the ceramic piece, the ceramic piece is always soaked in the surfactant, so that the liquid can be more favorably infiltrated into the gaps between the grain boundaries of the ceramic piece, and the particles hidden in the gaps can be cleaned and removed.
It should be noted that, soaking the ceramic piece in the surfactant, wiping the ceramic piece until the whole surface is wiped, and the process is 1 st time; the ceramic piece is then re-soaked in unused surfactant and wiped until the entire surface is wiped, 2 nd time, and so on.
A detailed description will be given below of a specific embodiment of the third cleaning process described above. Specifically, as shown in fig. 4, the third cleaning process specifically includes the following steps:
s301, soaking the ceramic piece subjected to the second cleaning process in deionized water, and performing ultrasonic cleaning;
optionally, in step S301, the resistivity of the deionized water is in a range of 2M Ω · cm or more, and the cleaning time is in a range of 10min or more and 15min or less.
The step S301 can be used for comprehensively cleaning the ceramic piece, and the cleaning effect of ultrasonic cleaning by using deionized water is most obvious, so that after the ultrasonic cleaning step is completed, the cleaning effect of the ceramic piece can be ensured to meet the process requirement. Further, the removal of particles on the surface of the ceramic piece and fine particles in the gaps between the grain boundaries of the ceramic piece has been achieved by the foregoing first cleaning process and second cleaning process, so that 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;
the resistivity of the deionized water used in the step S302 is higher than the resistivity of the deionized water used in the step S301, for example, the resistivity of the deionized water in the step S301 is in a range of 2M Ω · cm or more, and the resistivity of the deionized water in the step S302 is in a range of 4M Ω · cm or more.
The temperature of the deionized water used in the step S302 is higher than that of the deionized water used in the step S301. For example, the temperature of the deionized water used in the step S302 is normal temperature (generally 25 ℃), and the temperature of the deionized water used in the step S301 is in a range of 32 ℃ or higher and 42 ℃ or lower.
In order to improve the cleaning effect, optionally, in the soaking process, new deionized water is always introduced into the cleaning tank, and the deionized water in the cleaning tank is discharged in an overflow mode, so that the deionized water can be in a circulating flow state, and the cleaning effect can be further improved.
S303, sweeping the soaked ceramic piece, and baking the ceramic piece after sweeping.
Optionally, the purge gas adopted in step S303 includes nitrogen, and the purity of the nitrogen is 99.999%; the angle between the purging direction of the nitrogen gas and the surface of the ceramic piece ranges from 30 ° or more to 45 ° or less, for example, to prevent particles from falling again on the surface of the ceramic piece.
Optionally, firstly, completely purging the ceramic piece by using dry nitrogen; then purging the purification furnace (or oven) with dry nitrogen gas to dry the inside thereof; finally, the ceramic piece is put into a purging purification furnace (or an oven) for baking.
Next, a comparative experiment will be performed on the ceramic parts obtained by the ceramic part cleaning method in the prior art and the ceramic part cleaning method provided in the embodiment of the present invention. Specifically, the ceramic part cleaning method in the prior art comprises the following steps: firstly, soaking the ceramic piece in an alkaline degreasing agent for 50-80 min, and then putting the ceramic piece into deionized water for rinsing (spraying pressurized deionized water on all parts of the surface of the ceramic piece); and then, immersing the ceramic piece in an acid solution for 5min-10min, taking out the ceramic piece from the solution, immersing the ceramic piece in deionized water again for rinsing, immersing the ceramic piece in deionized water with the resistivity rate of more than or equal to 4M omega cm and normal temperature for ultrasonic cleaning for 10min-15min, immersing the ceramic piece in deionized water with the resistivity of more than or equal to 8M omega cm for hot water immersion cleaning, finally, blowing the ceramic piece dry by using nitrogen, and drying the ceramic piece, thereby completing the whole cleaning process.
The ceramic part cleaning method provided by the embodiment of the invention comprises the three cleaning processes, wherein the first cleaning process comprises the steps S101-S106; the second cleaning process comprises soaking the sprayed ceramic piece in the surfactant, and wiping the whole surface of the ceramic piece in the surfactant for at least 3 times; the third cleaning process includes the above-described steps S301 to S303.
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 scanning image of the ceramic part obtained by the ceramic part cleaning method according to the embodiment of the present invention. As can be seen from comparing fig. 5 and fig. 6, the ceramic article obtained by the ceramic article cleaning method in the prior art still has suspended particles on the surface, as shown in fig. 5 (a) and (b), and the white dots on the black area are the suspended particles. In addition, the ceramic part obtained by the ceramic part cleaning method in the prior art has the particle number per unit area of more than or equal to 50ea which is far higher than the particle index (the particle number per unit area is less than 2ea) and falls on the wafer in the process. In contrast, as can be seen from the graphs (a) and (b) in fig. 6, the white dots on the black area in the graph are significantly reduced, so that it can be seen that the suspended particles on the ceramic article obtained by the ceramic article cleaning method provided by the embodiment of the present invention are significantly reduced, and the number of particles per unit area of the ceramic article falling on the wafer during the process is lower than the particle index (the number of particles per unit area is less than 2 ea).
The ceramic member in the present embodiment includes, for example, a ceramic process kit for a semiconductor apparatus. The ceramic process kit can be parts such as a lining, a medium window, a nozzle, a sieve tube, a main medium cylinder and an auxiliary medium cylinder of a three-dimensional induction coil, an observation window protection cylinder and the like which are made of ceramic materials.
In summary, the cleaning method for the ceramic part provided by the embodiment divides the 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 on the blind holes, folds and non-welding seams with larger sizes on the surface of the ceramic part; in the second cleaning process, the whole surface of the ceramic part is cleaned by adopting the surfactant provided by the embodiment, so that tiny particles hidden in gaps among crystal boundaries of the ceramic can be effectively removed; the third cleaning process adopts an ultrasonic cleaning mode to clean the ceramic piece so as to remove residual particles and solution (acid or alkaline solution) on the ceramic piece, so that the ceramic piece can be comprehensively cleaned, and finally, the cleaning effect can be effectively improved.
It will be understood that the above embodiments are merely exemplary embodiments taken to illustrate the principles of the present invention, which is not limited thereto. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit and substance of the invention, and these modifications and improvements are also considered to be within the scope of the invention.
Claims (15)
1. A surfactant for removing particles from a ceramic article, the surfactant comprising: deionized water, organic phosphoric acid scale and corrosion inhibitors, a first organic compound for improving the detergency and the dispersibility of the surfactant, a second organic compound for removing oil dirt on the surface of the ceramic part, polymerized phosphate, alkyl organic compounds and an acidic solution.
2. The surfactant according to claim 1, wherein the deionized water is 10000 parts by weight; 9-11 parts of an organic phosphoric acid scale and corrosion inhibitor; 15-17 parts of the first organic compound; 9-11 parts of a second organic compound; 9-11 parts of polymerized phosphate; 14-16 parts of alkyl organic compound; and 9-11 parts of the acidic solution.
3. The surfactant according to claim 1 or 2, wherein the organic phosphoric acid-based 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 a succinate phosphate; the alkyl organic compound comprises sodium alkyl benzene sulfonate; the acidic solution comprises a hydrogen chloride solution.
4. The surfactant according to claim 3, 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 alkyl benzene sulfonate; the hydrogen chloride solution is 10 parts.
5. The surfactant according to claim 3, wherein the concentration of hydrogen chloride in the hydrogen chloride solution is 40% to 60%.
6. A method for producing a surfactant, which is used for producing the surfactant according to any one of claims 1 to 5; 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 polymeric phosphate, the alkyl organic compound and the acidic solution into the reaction vessel in time sequence, and stirring the solution in the reaction vessel in the process of adding each component.
7. The method for preparing a surfactant according to claim 6, 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.
8. The method according to claim 7, wherein the time for stirring the solution in the reaction vessel after adding each of the components and before adding the next component is 3min or more and 5min or less.
9. The method according to claim 6, wherein in step S2, the solution in the reaction vessel is stirred by 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.
10. The method according to claim 6, wherein the temperature of the deionized water in step S1 is 42 ℃ or higher and 50 ℃ or lower.
11. A method of cleaning a ceramic part, comprising:
a first cleaning process, wherein particles on the ceramic piece are dissolved by adopting a chemical solution;
a second cleaning process of cleaning the entire surface of the ceramic piece with the surfactant according to any one of claims 1 to 5 to remove fine particles;
and in the third cleaning process, the ceramic piece is cleaned in an ultrasonic cleaning mode to remove residual particles and solution on the ceramic piece.
12. A method for cleaning ceramic parts according to claim 11, characterized in that the first cleaning process comprises in particular the following steps:
s101, soaking the 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 soaked in the deionized water;
s104, soaking the sprayed ceramic piece in an acid solution;
s105, soaking the ceramic piece soaked in the acidic solution in deionized water;
and S106, spraying the deionized water with the specified pressure on the whole surface of the ceramic piece soaked in the deionized water.
13. A method for cleaning ceramic parts according to claim 11, wherein the second cleaning process comprises:
immersing the ceramic piece having completed the first cleaning process in the surfactant, and wiping the entire surface of the ceramic piece in the surfactant at least 3 times.
14. A method for cleaning ceramic parts according to claim 11, characterized in that the third cleaning process comprises the following steps:
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, sweeping the cleaned ceramic piece, and baking the ceramic piece after sweeping.
15. A method for cleaning ceramic parts according to any one of claims 11-14, wherein the ceramic parts comprise ceramic process kits for semiconductor equipment.
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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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| Country | Link |
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| CN (1) | CN113414167B (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022267916A1 (en) * | 2021-06-23 | 2022-12-29 | 北京北方华创微电子装备有限公司 | Surfactant, preparation method therefor, and method for cleaning ceramic part |
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Also Published As
| Publication number | Publication date |
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| TWI813333B (en) | 2023-08-21 |
| CN113414167B (en) | 2023-08-18 |
| WO2022267916A1 (en) | 2022-12-29 |
| TW202300636A (en) | 2023-01-01 |
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